CN103018378B - 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 blowback principle, gas chromatograph with gas-oil separation function and measure the process of gas chromatography of micro-moisture in insulating oil.
Background technology
Power industry generally adopts insulating oil to ensure the insulation between associated components in transformer and sleeve pipe.And along with the operation of these equipment, in oil, can sneak into some micro-moistures, and then greatly reduce the insulating property of insulating oil, shorten the normal service life of transformer and sleeve pipe, also may cause the generation of some accidents, cause huge loss and harm.Therefore, the micro-water monitoring in 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 to clear and definite regulation in standard, and GB/T 7601 is also 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 gas-oil separation function as vaporizer.Under normal circumstances, to the requirement of this injector be: 1. can withstand long term exposure the high temperature of 200 DEG C; 2. material used can allow hydrone freely see through, and oil sample can be by effectively catching in injector; 3. after each oil-feed sample, Residual oil must be discharged injector in time, in case cause that profit interacts, affects micro-instant water gasification, and in this process, can not affect the impermeability of air-channel system; 4. the injector internal volume of water molecule energy contact is as far as possible little, otherwise Wei Shui peak type broadening, cannot be quantitative.Due to high to injector performance requirement, on market, also do not have thisly under hot conditions, can moment effectively realize the microsyringe of oil-water separating function.And adopt general gas chromatograph, only sample introduction several times, just makes chromatographic column severe contamination, even pollutes conductance cell, not only makes to measure to carry out, and also can damage valuable chromatograph.
Summary of the invention
The technical problem to be solved in the present invention be to provide a kind of gas circuit structure simple, be easy to manufacture and effective, the gas chromatograph with gas-oil separation function based on blowback principle of gas-oil separation function, and a kind of process of gas chromatography of measuring micro-moisture in 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 gas-oil separation function, in its gas circuit structure, contain thermal conductivity detector (TCD) (TCD), analyze chromatographic column, 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 corresponding tracheae or passage, needle valve, the reference arm of thermal conductivity detector (TCD), six-way valve interface 1., six-way valve interface 2., injector, protection chromatographic column, six-way valve interface 5., 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 corresponding tracheae or passage, pressure maintaining valve B, six-way valve interface 4. with connect open to atmosphere six-way valve interface 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, in described sample cavity, be filled with carrier, 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 after this exhausr port, be connected to solenoid valve B, 2. described air intake opening is connected to described six-way valve interface via corresponding pipeline, the lower end of this injector is connected with described protection chromatographic column via corresponding pipeline, while 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 be 6. connected respectively, while carrying out gas circuit blowback, described solenoid valve A and B open, 1. and 6. and described six-way valve interface, and 3. 2., 4. and be 5. connected, 5. 4. the high-purity carrier gas that makes to flow out from described T-valve pass through solenoid valve A, pressure maintaining valve B, six-way valve interface and successively, then enter successively emptying after described protection chromatographic column, injector and form blowback gas circuit, and then described protection chromatographic column, injector are carried out to reverse blow.
The process of gas chromatography that utilizes micro-moisture in 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 DEG C, include described protection chromatographic column and analyze chromatographic column is 120～150 DEG C, the conductance cell temperature of thermal conductivity detector (TCD) is 150～160 DEG C, described six-way valve temperature is 100～120 DEG C, carrier gas (high pure nitrogen or helium) flow velocity 28～32mL/min;
(2) described in pass, close solenoid valve A and B, 1. and 2. make respectively described six-way valve interface, and 4. 3., 5. and be 6. connected, inject fast testing sample from the injection port of injector, enter and detect gas circuit through 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. 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. six-way valve interface, analyze chromatographic column, the gage beam that enters thermal conductivity detector (TCD) detects, 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 six-way valve connecting interface, 1. and 6. make described six-way valve interface, and 3. 2., 4. and be 5. connected respectively, 5. 4. the high-purity carrier gas that makes to flow out from described T-valve pass through solenoid valve A, pressure maintaining valve B, six-way valve interface and successively, enter successively more emptying after described protection chromatographic column, injector and form blowback gas circuit, and then described protection chromatographic column, injector are carried out to reverse blow;
(4) flow out the gage beam of TCD completely 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 through deactivation processing.
Described protection chromatographic column or the filler of analyzing in chromatographic column are at least one in GDX502, GDX301, GDX102.
Described protection chromatographic column and analysis chromatographic column are all arranged in 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:
(1) can ensure to analyze time, moisture peak type be unaffected, can make again entered oil sample and oil vapour be gone out chromatographic system by blowback in time, avoids Residual oil contamination analysis post and detector cell body.
(2) designed injection port structure, can effectively ensure sample introduction time, the oil sample of difficult gasification is trapped in injection port; And when blowback, be convenient to Residual oil and discharge smoothly chromatographic system.
(3) gas circuit structure is simple, and the injector that directly carries out gas-oil separation than high temperature is easy to manufacture, and realizes the successful of gas-oil separation function; The good airproof performance of entire system.
Brief description of the drawings
Fig. 1 is the process of gas chromatography figure under sample introduction state;
Fig. 2 is the injector assembling flow path figure under analysis state;
Fig. 3 is the structural representation of injector used in the gas circuit of gas chromatograph of the present invention;
Fig. 4 is certain result collection of illustrative plates of micro-moisture in gas chromatograph for determination insulating oil of the present invention.
In figure, 1 is T-valve, and 2 is pressure maintaining valve A, and 3 is needle valve, 4 reference arms that are thermal conductivity detector (TCD); 5 is six-way valve, and 6 is injector, and 7 is protection chromatographic column, and 8 for analyzing chromatographic column; 9 is the gage beam of thermal conductivity detector (TCD), and 10 is pressure maintaining valve B, and 11 is solenoid valve A, 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 in following embodiment, if no special instructions, be conventional method.
1 one kinds of the embodiment gas chromatograph with gas-oil separation function, referring to Fig. 1, Fig. 2, Fig. 3, contains thermal conductivity detector (TCD) in its gas circuit structure, analyze chromatographic column 8(internal diameter 2mm, column length is not less than 1.8m, adopts porous polymer bead class filler, as GDX502, and GDX301 or GDX102), protection chromatographic column 7(internal diameter 2mm, column length is 1/10th left and right of analytical column, adopts porous polymer bead class filler, as GDX502, GDX301 or GDX102), six-way valve 5, injector 6, T-valve 1, pressure maintaining valve A 2 and pressure maintaining valve B 10, be with manometric needle valve 3, solenoid valve A 11 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, and described detection gas circuit connects pressure maintaining valve A 2 successively via corresponding tracheae or passage, 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 corresponding tracheae or passage connected electromagnetic valve A 11 successively, pressure maintaining valve B 10, six-way valve 5 interfaces 4. with connect open to atmosphere six-way valve 5 interfaces 3. form, while carrying out sample determination, solenoid valve A 11 and solenoid valve B 22 close, and six-way valve 5 interfaces 1. and 2., 3. and 4., 5. and be 6. connected respectively, while carrying out gas circuit blowback, solenoid valve A 11 and solenoid valve B 22 open, and six-way valve 5 interfaces 1. with interface 6., 2. and 3., 4. and be 5. connected respectively, in this state, injector 6 and protection chromatographic column 7 are in blowback state.The switching mode of six-way valve can adopt pneumatic or motorized motions, but generally, 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 interior steel pipe 18(internal diameter 4～5mm wherein, the stainless-steel tube of length 30～40mm) be distinguished into sample cavity 14 and exocoel 19 two parts, in sample cavity 14, be filled with carrier (can be glass microsphere carrier or other Diatomaceous Earth Support through deactivation processing of silanization), 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 after this exhausr port 18, 2. air intake opening 17 is connected to six-way valve 5 interfaces via corresponding pipeline, the lower end of this injector is connected with protection chromatographic column 7 via corresponding pipeline, sample injects from the openend 15 of injection port top with micro-injection pin, and in the gasification of the upper end of sample cavity 14.
TCD detecting device in gas circuit is highly sensitive pair of pond four arm detecting devices, does in carrier gas situation at nitrogen, can be less than 0.5ppm to the sensitivity of micro-water.
In described process of gas path, TCD pond body is arranged in the environment that can keep constant high temperature; injector 6 temperature at least can be heated to 200 DEG C; six-way valve 5 in being not less than the environment of 100 DEG C, protection chromatographic column 7 and analyze chromatographic column 8 and be arranged in post case, post case temperature should be able to free setting.
The process of gas chromatography that utilizes micro-moisture in 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 DEG C, include described protection chromatographic column and analyze chromatographic column is 120 DEG C, the conductance cell temperature of thermal conductivity detector (TCD) is 150 DEG C, described six-way valve temperature is 100 DEG C, carrier gas (high pure nitrogen) flow velocity 30mL/min;
(2) described in pass, close solenoid valve A and B, 1. and 2. make respectively described six-way valve interface, and 4. 3., 5. and be 6. connected, inject fast testing sample from the injection port of injector, enter and detect gas circuit through 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. 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. six-way valve interface, analyze chromatographic column, the gage beam that enters thermal conductivity detector (TCD) detects (testing result is referring to Fig. 4), 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 six-way valve connecting interface, 1. and 6. make described six-way valve interface, and 3. 2., 4. and be 5. connected respectively, 5. 4. the high pure nitrogen that makes to flow out from described T-valve pass through solenoid valve A, pressure maintaining valve B, six-way valve interface and successively, enter successively more emptying after described protection chromatographic column, injector and form blowback gas circuit, and then described protection chromatographic column, injector are carried out to reverse blow;
(4) flow out the gage beam of TCD completely 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 in GB GB/T 7601-2008 need have 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 without departing from theon the basis of the spirit of the present invention, all belong to the scope of protection of present invention.
Claims (8)
1. the gas chromatograph with gas-oil separation function, in its gas circuit structure, contain thermal conductivity detector (TCD), analyze chromatographic column, 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 corresponding tracheae or passage, needle valve, the reference arm of thermal conductivity detector (TCD), six-way valve first interface (1.), six-way valve the second interface (2.), injector, protection chromatographic column, six-way valve the 5th interface (5.), six-way valve the 6th 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 corresponding tracheae or passage, pressure maintaining valve B, six-way valve the 4th interface (4.) and connect open to atmosphere six-way valve the 3rd interface (3.) and forming, 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, in described sample cavity, be filled with carrier, 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 of outwards arranging Residual oil for described exocoel, and after this exhausr port, be connected to solenoid valve B, described air intake opening is connected to described six-way valve the second interface (2.) via corresponding pipeline, the lower end of this injector is connected with described protection chromatographic column via corresponding pipeline, while carrying out sample determination, described solenoid valve A and solenoid valve B close, and described six-way valve first interface (1.) and the second interface (2.), the 3rd interface (3.) and the 4th interface (4.), the 5th interface (5.) and the 6th interface (6.) are connected respectively, while carrying out gas circuit blowback, described solenoid valve A and solenoid valve B open, and described six-way valve first interface (1.) and the 6th interface (6.), the second interface (2.) and the 3rd interface (3.), the 4th interface (4.) and the 5th interface (5.) are 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 the 4th interface (4.) and the 5th interface (5.), enter successively more emptying after described protection chromatographic column, injector and form blowback gas circuit, and then described protection chromatographic column, injector are carried out to reverse blow.
2. the gas chromatograph with gas-oil separation function according to claim 1, is characterized in that, the glass microsphere carrier that the carrier that described sample cavity is filled is silanization or the Diatomaceous Earth Support through deactivation processing.
3. the gas chromatograph with gas-oil separation function according to claim 1, is characterized in that, described protection chromatographic column or the filler of analyzing in chromatographic column are at least one in GDX502, GDX301, GDX102.
4. the gas chromatograph with gas-oil separation function according to claim 1; it is characterized in that; described protection chromatographic column and analysis chromatographic column are all arranged in 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 described in claim 1 process of gas chromatography of micro-moisture in gas chromatograph for determination insulating oil, comprising:
(1) the post case temperature that to set the vaporizer temperature of gas chromatograph sampling device described in claim 1 be 180～220 DEG C, include described protection chromatographic column and analyze chromatographic column is 120～150 DEG C, the conductance cell temperature of thermal conductivity detector (TCD) is 150～160 DEG C, described six-way valve temperature is 100～120 DEG C, and carrier gas high pure nitrogen flow velocity is 28～32ml/min;
(2) described in pass, close solenoid valve A and B, make respectively described six-way valve first interface (1.) and the second interface (2.), the 3rd interface (3.) and the 4th interface (4.), the 5th interface (5.) and the 6th interface (6.) are connected, inject fast testing sample from the injection port of injector, enter and detect gas circuit through 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, after six-way valve first interface (1.) and the second interface (2.), enter described injector, and carry the vaporized composition to be measured described protection chromatographic column of flowing through successively, six-way valve the 5th interface (5.) and the 6th interface (6.), analyze chromatographic column, the gage beam that enters thermal conductivity detector (TCD) detects, tail gas is emptying,
(3) when described composition to be measured flows through after described six-way valve the 6th interface (6.), described solenoid valve A and B open simultaneously, and switch six-way valve connecting interface, make described six-way valve first interface (1.) and the 6th interface (6.), the second interface (2.) and the 3rd interface (3.), the 4th interface (4.) and the 5th interface (5.) are connected respectively, make the high pure nitrogen flowing out from described T-valve pass through successively solenoid valve A, pressure maintaining valve B, six-way valve the 4th interface (4.) and the 5th interface (5.), enter successively more described protection chromatographic column, emptying and form blowback gas circuit after injector, and then to described protection chromatographic column, injector carries out reverse blow,
(4) when composition to be measured divides the gage beam that flows out thermal conductivity detector (TCD) completely, and after baseline is steady, 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 mensuration insulating oil according to claim 5, is characterized in that, the glass microsphere carrier that the carrier that described sample cavity is filled is silanization or the Diatomaceous Earth Support through deactivation processing.
7. the process of gas chromatography of micro-moisture in mensuration insulating oil according to claim 5, is characterized in that, described protection chromatographic column or the filler of analyzing in chromatographic column are at least one in GDX502, GDX301, GDX102.
8. the process of gas chromatography of micro-moisture in mensuration insulating oil according to claim 5; it is characterized in that; described protection chromatographic column and analysis chromatographic column are all arranged in 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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| 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 |
| CN104297388B (en) * | 2014-10-23 | 2016-08-24 | 佛山市南海区环境保护监测站 | Sampling device |
| 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 |
| 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 |
| 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 |
| CN112798723B (en) * | 2021-03-09 | 2023-04-11 | 郑州大学 | Quantitative analysis device for detecting gas chromatograph blowback gas |
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