CN117310011A - Be applicable to SF 6 Helium ion gas chromatograph for detecting decomposition products - Google Patents
Be applicable to SF 6 Helium ion gas chromatograph for detecting decomposition products Download PDFInfo
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- CN117310011A CN117310011A CN202311021432.6A CN202311021432A CN117310011A CN 117310011 A CN117310011 A CN 117310011A CN 202311021432 A CN202311021432 A CN 202311021432A CN 117310011 A CN117310011 A CN 117310011A
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- 239000007789 gas Substances 0.000 title claims abstract description 197
- 229910052734 helium Inorganic materials 0.000 title claims abstract description 39
- 239000001307 helium Substances 0.000 title claims abstract description 39
- 238000000354 decomposition reaction Methods 0.000 title claims abstract description 21
- 239000012159 carrier gas Substances 0.000 claims abstract description 94
- 238000001179 sorption measurement Methods 0.000 claims abstract description 71
- 238000001536 pulsed discharge helium ionisation detection Methods 0.000 claims abstract description 44
- 238000003860 storage Methods 0.000 claims abstract description 26
- -1 helium ion Chemical class 0.000 claims abstract description 25
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000002808 molecular sieve Substances 0.000 claims abstract description 20
- 238000010438 heat treatment Methods 0.000 claims abstract description 17
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000000926 separation method Methods 0.000 claims abstract description 8
- 238000003795 desorption Methods 0.000 claims abstract description 4
- 238000001514 detection method Methods 0.000 claims description 44
- 238000010926 purge Methods 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 19
- 238000011144 upstream manufacturing Methods 0.000 claims description 11
- 238000004458 analytical method Methods 0.000 claims description 8
- 238000005086 pumping Methods 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 3
- 229910018503 SF6 Inorganic materials 0.000 description 24
- SFZCNBIFKDRMGX-UHFFFAOYSA-N sulfur hexafluoride Chemical compound FS(F)(F)(F)(F)F SFZCNBIFKDRMGX-UHFFFAOYSA-N 0.000 description 24
- 229960000909 sulfur hexafluoride Drugs 0.000 description 23
- 230000035945 sensitivity Effects 0.000 description 8
- 239000012535 impurity Substances 0.000 description 4
- 239000003463 adsorbent Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/08—Preparation using an enricher
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/12—Preparation by evaporation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/64—Electrical detectors
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/08—Preparation using an enricher
- G01N2030/085—Preparation using an enricher using absorbing precolumn
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/12—Preparation by evaporation
- G01N2030/125—Preparation by evaporation pyrolising
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention describes a SF applicable 6 The helium ion gas chromatograph for detecting decomposition products is characterized in that the sample gas in a quantitative ring is led into a later stage adsorption column through carrier gas, the adsorption column contains enough kdhf-0 type molecular sieve, and the sample gas and the carrier gas are kept stand in the adsorption column for a set time, and then SO is carried out 2 The gas is completely absorbed, and the carrier gas is reused to absorb the gas and only contains helium and SF 6 The gas is purged to the post chromatographic column for separation, a heating rod in the adsorption column is started after a set time period, the molecular sieve is heated to 100 ℃ for desorption, and the desorbed SO is desorbed by carrier gas 2 After the gas is led into the small gas storage tank and the set time length, the valve is controlled to stop the carrier gas from entering the adsorption column and startThe residual gas in the adsorption column is pumped into the gas storage tank by the dynamic vacuum pump, then the vacuum pump is stopped, the valve is controlled again to flow the carrier gas through the adsorption column, the gas in the gas storage tank is pushed to enter the post-stage chromatographic column, and SO in the gas is generated 2 The gas enters a PDHID detector, and under the condition of no SF6 gas interference, the ultra-low concentration SO is accurately detected 2 Gas concentration.
Description
Technical Field
The invention relates to the technical field of gas detection, in particular to a gas sensor suitable for SF 6 Helium ion gas chromatograph for detecting decomposition products.
Background
Sulfur hexafluoride (SF) 6 ) Is the most ideal insulating and arc extinguishing medium in all substances in nature and artificial synthesis at present, although the Global Warming Potential (GWP) is CO 2 Is 23900 times that of the power system, but is still widely used in the power system. SF (sulfur hexafluoride) 6 The gas can generate trace toxic corrosive gas such as SO with other substances under the action of latent faults such as discharge or overheat 2 、SOF 2 (fluorosulfinyl), H 2 S, CO, etc., damage the insulating material and further cause more serious failures. In the electric power system, whether the electrical equipment has latent faults and fault types are often judged by detecting decomposition products, and then corresponding defending measures are selected. SO (SO) 2 As the most prominent characteristic decomposition product, its concentration is generally used as the primary basis for judging latent faults by on-site operators.
At present, detection of SF6 gas decomposition products is mainly divided into field detection and laboratory detection, wherein the laboratory detection precision and sensitivity are obviously higher than those of the field detection. Early in the occurrence of latent faults, SO 2 The concentration may be only a few hundred ppb (parts per billion by volume) to a few ppm (parts per million by volume), SO that it is difficult for in-situ detection instruments to detect SO at such low concentrations 2 . Thus, for very low concentrations of SO 2 The detection instrument generally adopts a laboratory detection instrument-gas chromatograph. The gas chromatograph can be classified into a thermal conductivity method, a sulfur chemiluminescence method, a helium ion method, and the like according to the difference of detectors, wherein the helium ion gas chromatograph is widely applied to the analysis work of ultra-low concentration gas impurities due to extremely high detection sensitivity. Helium ion gas chromatographyThe basic detection principle of the instrument is that gas which is separated by a chromatographic column and flows out in sequence is led into a helium ion detector (PDHID) through a cut valve technology, helium is electrolyzed into high-energy metastable helium ions by PDHID through an electric arc generated by discharge, and the high-energy helium ions are utilized to ionize gas components to be detected, so that the concentration detection of impurity gas is realized. However, SF is performed 6 Gas decomposition product SO 2 During gas detection, SF in sample gas 6 The concentration ratio is generally above 99%, and SF is sequentially discharged after separation by chromatographic column 6 And SO 2 It is difficult to completely separate the two by a cut valve. Once there is a small amount of SF 6 Gas and SO 2 The gas enters the PDHID detector together, and the arc generated by PDHID discharge is rapidly subjected to SF with excellent arc extinguishing capability 6 The gas is extinguished, helium is not fully ionized into high-energy metastable helium ions, thereby affecting SO 2 As a result of ionization of the gas, the detection sensitivity and accuracy are reduced.
Therefore, there is a need to study the corresponding technology to solve the SF in the prior art 6 Influence of gas on helium ion gas chromatography PDHID detector, and improvement of analysis SF 6 Gas decomposition product SO 2 The sensitivity and accuracy of detection at gas concentrations.
Disclosure of Invention
The invention aims at solving the technical problem of how to detect SF by adopting a helium ion gas chromatograph 6 Gas decomposition product SO 2 SF when 6 The gas has an arc extinguishing effect on the discharge arc of the PDHID detector, influences helium ionization, and reduces detection sensitivity and precision.
The invention solves the technical problems by the following technical means:
be applicable to SF 6 The helium ion gas chromatograph for detecting the decomposition products comprises a six-way valve, a quantitative ring, an adsorption column, a vacuum pump, a gas storage tank, a chromatographic column, a PDHID detector and first to eleventh electromagnetic valves;
the carrier gas inlet is communicated with the carrier gas inlet of the six-way valve, the carrier gas outlet of the six-way valve is communicated with the inlet of the adsorption column, and the outlet of the adsorption column is communicated with the inlet of the chromatographic column; the outlet of the chromatographic column is communicated with the inlet of the PDHID detector; the carrier gas inlet is communicated with the inlet of the PDHID detector;
a first electromagnetic valve is connected in series between the carrier gas inlet and the carrier gas inlet of the six-way valve; a tenth electromagnetic valve is connected in series between the carrier gas inlet and the PDHID detector; a third electromagnetic valve, a seventh electromagnetic valve and a ninth electromagnetic valve are sequentially connected in series between the adsorption column and the chromatographic column; the upstream of the ninth electromagnetic valve is connected with the upstream of the tenth electromagnetic valve in series through an eighth electromagnetic valve; a second electromagnetic valve, a vacuum pump, a fifth electromagnetic valve, a gas storage tank and a sixth electromagnetic valve are connected in series between the outlet of the adsorption column and the upstream of the ninth electromagnetic valve in sequence; and a fourth electromagnetic valve is connected in series between the downstream of the third electromagnetic valve and the outlet of the vacuum pump. The invention introduces the sample gas in the quantitative ring into the post-stage adsorption column through the carrier gas, the adsorption column contains enough kdhf-0 type molecular sieve, and the sample gas and the carrier gas are kept stand in the adsorption column for a set time, and then SO 2 The gas is completely absorbed, and the carrier gas is reused to absorb the gas and only contains helium and SF 6 The gas is purged to the post chromatographic column for separation, a heating rod in the adsorption column is started after a set time period, the molecular sieve is heated to 100 ℃ for desorption, and the desorbed SO is desorbed by carrier gas 2 After the set time, the valve is controlled to enable the carrier gas to suspend entering the adsorption column, the vacuum pump is started to pump all residual gas in the adsorption column into the gas storage tank, then the vacuum pump is stopped, the valve is controlled again to enable the carrier gas to flow through the adsorption column, the gas in the gas storage tank is pushed to enter the post-stage chromatographic column, and SO in the gas 2 The gas enters a PDHID detector in the absence of SF 6 Under the condition of gas interference, accurately detecting ultralow concentration SO 2 Gas concentration.
The invention adopts the adsorbent to carry out SO 2 The gas is adsorbed and desorbed, thereby separating SO 2 And SF (sulfur hexafluoride) 6 Complete separation of SO 2 After SF 6 Enters the chromatographic column, thereby avoiding the detection of SO by a PDHID detector 2 When there is a small amount of SF 6 Gas, reducing detection sensitivity and accuracy.
Furthermore, a check valve is connected in series to the exhaust pipe of the PDHID detector.
Further, an eleventh electromagnetic valve is arranged on an exhaust pipeline of the vacuum pump.
Further, the adsorption column comprises a molecular sieve and a heating rod, and the heating rod heats the molecular sieve.
Further, the detection method comprises the following steps:
step three, vacuumizing;
purging;
after purging, the six-way valve communicates the sample gas inlet with the quantitative ring inlet through the cut valve, the sample gas enters the quantitative ring, after quantitatively collecting a certain volume of gas, the six-way valve connects the carrier gas inlet, the quantitative ring outlet and the carrier gas outlet in sequence through the cut valve, and the carrier gas brings the sample gas in the quantitative ring into the subsequent adsorption column;
after the carrier gas containing the sample gas enters the adsorption column, all electromagnetic valves are closed at the moment, the gas is stored in the adsorption column, and the carrier gas is kept stand for a set period of time until SO 2 After the gas is fully adsorbed, the third electromagnetic valve, the seventh electromagnetic valve and the ninth electromagnetic valve are opened at the moment, and only helium and SF are contained 6 The gas enters a post-stage chromatographic column, is separated by the chromatographic column, enters a post-stage PDHID detector, and is discharged to the outside from a detection gas outlet after detection and analysis;
after the third electromagnetic valve is opened for a set period of time, SF in the adsorption column 6 The gas is completely pushed out by the carrier gas and enters the chromatographic column, at the moment, the third electromagnetic valve and the seventh electromagnetic valve are closed, the six-way valve disconnects the carrier gas inlet from the quantitative ring through the cut valve, and the carrier gas enters the carrier gas inlet and is directly discharged; at this time, the eighth electromagnetic valve is opened, and the carrier gas continuously enters the chromatographic column; then, starting a heating rod in the adsorption column to heat to a set temperature, then opening a second electromagnetic valve and a fifth electromagnetic valve, starting a vacuum pump, and desorbing SO 2 Pumping into a gas storage tank, vacuumizing for a set period of time, and adsorbing all SO in the column 2 The gas is pumped to the gas storage tank, the vacuum pump is closed at the moment, the second electromagnetic valve, the seventh electromagnetic valve and the eighth electromagnetic valve are closed, the third electromagnetic valve, the fourth electromagnetic valve, the fifth electromagnetic valve and the sixth electromagnetic valve of the electromagnetic valves are opened, and the six-way valve cuts off the valve to enable the carrier gas inlet and the carrier gasThe outlets are communicated, and the carrier gas continuously pushes SO in the gas storage tank 2 The gas enters a post chromatographic column, passes through a PDHID detector, is discharged to the outside from a detected gas outlet after detection and analysis, and waits for SO to appear 2 And after the detection result, closing all electromagnetic valves, stopping air inlet, and ending the detection process.
Further, the specific method for vacuumizing comprises the following steps: opening the vacuum pump, opening the second electromagnetic valve, the third electromagnetic valve, the sixth electromagnetic valve, the seventh electromagnetic valve and the eleventh electromagnetic valve, closing other electromagnetic valves, vacuumizing to a set value, closing the vacuum pump, and closing all the electromagnetic valves.
Further, the specific purging method in the step is as follows: the carrier gas enters from the carrier gas inlet, the first electromagnetic valve and the tenth electromagnetic valve are opened, one path of carrier gas flows to the carrier gas inlet of the six-way valve to purge the six-way valve, and the gas after purging is directly discharged; the other path of gas flows to the PDHID detector to purge the PDHID detector, and the purged gas is discharged to the outside from a detected gas outlet of the PDHID detector, and the tenth electromagnetic valve is closed after the purging is finished.
Further, the purging further comprises purging of the sample gas pipeline, specifically: sample gas enters the six-way valve from the sample gas inlet, and at the moment, the six-way valve is used for communicating the sample gas inlet with the sample gas outlet through the cut valve, so that the sample gas is discharged to the outside from the sample gas outlet, and the purging of the sample gas pipeline is realized.
Further, in the step, the heating rod heats the kdhf-0 type molecular sieve in the adsorption column to 100 ℃.
The invention has the advantages that:
this example uses an adsorbent to remove SO 2 The gas is adsorbed and desorbed, thereby separating SO 2 And SF (sulfur hexafluoride) 6 Complete separation of SO 2 After SF 6 Enters the chromatographic column, thereby avoiding the detection of SO by a PDHID detector 2 When there is a small amount of SF 6 Gas, reducing detection sensitivity and accuracy.
Drawings
Fig. 1 is a schematic diagram showing the overall structure of a helium ion gas chromatograph according to embodiment 1 of the present invention.
FIG. 2 is an enlarged view showing the structure of the adsorption column in example 1 of the present invention.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions in the embodiments of the present invention will be clearly and completely described in the following in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
As shown in fig. 1, this embodiment describes a method suitable for SF 6 The helium ion gas chromatograph for detecting the decomposition products comprises a six-way valve 7, a quantitative ring 8, an adsorption column 12, a vacuum pump 14, a gas storage tank 18, a chromatographic column 23, a PDHID detector 14 and first to eleventh electromagnetic valves;
the carrier gas inlet 9 is communicated with the carrier gas inlet 2 of the six-way valve, the carrier gas outlet 3 of the six-way valve is communicated with the inlet of the adsorption column, and the outlet of the adsorption column 12 is communicated with the inlet of the chromatographic column 23; the outlet of the chromatographic column 23 is communicated with the inlet of a PDHID detector 24; the carrier gas inlet 9 communicates with the inlet of the PDHID detector 24;
a first electromagnetic valve 10 is connected in series between the carrier gas inlet 9 and the carrier gas inlet 2 of the six-way valve; a tenth electromagnetic valve 27 is connected in series between the carrier gas inlet 9 and the PDHID detector 24; a third electromagnetic valve 15, a seventh electromagnetic valve 20 and a ninth electromagnetic valve 22 are sequentially connected in series between the adsorption column 12 and the chromatographic column 23; upstream of the ninth electromagnetic valve 22 and upstream of the tenth electromagnetic valve 27 are connected in series through the eighth electromagnetic valve 21; a second electromagnetic valve 13, a vacuum pump 14, a fifth electromagnetic valve 17, a gas storage tank 18 and a sixth electromagnetic valve 19 are also connected in series in sequence between the outlet of the adsorption column 12 and the upstream of the ninth electromagnetic valve 22; a fourth electromagnetic valve 16 is also connected in series between the downstream of the third electromagnetic valve 15 and the outlet of the vacuum pump 14.
A non-return valve 25 is also connected in series upstream of the detector outlet 26 of the PDHID detector 24. An eleventh electromagnetic valve 28 is also connected in series upstream of the vacuum exhaust port 30 of the vacuum pump 14, and a vacuum gauge 29 is also installed on the vacuum exhaust port 30.
In this embodiment, the adsorption column 12 is further provided with a temperature sensor 11. The adsorption column 12 contains a sufficient amount of kdhf-03 type molecular sieve 122, and the molecular sieve 122 has good SO 2 Adsorption performance on SF 6 And helium gas has no adsorption capacity. The molecular sieve 122 has a columnar structure, the central through hole is provided with a heating rod 121, and the heating rod 121 is electrically heated and is used for heating the molecular sieve 122 SO as to desorb SO 2 。
In operation of this example, the sample gas (containing SO) in the dosing ring was dosed by a carrier gas (helium) 2 SF of impurities 6 Gas) is introduced into a post-stage adsorption column, the adsorption column contains enough kdhf-03 type molecular sieve, and the molecular sieve has good SO 2 Adsorption performance on SF 6 And helium gas has no adsorption capacity. Standing the sample gas and carrier gas in an adsorption column for 3min, and collecting SO 2 The gas is completely absorbed, and the carrier gas is reused to absorb the gas and only contains helium and SF 6 The gas is purged to the post chromatographic column for separation, a heating rod in the adsorption column is started after about 1min, the molecular sieve is heated to 100 ℃ for desorption, and the desorbed SO is desorbed by carrier gas 2 Introducing gas into a small-sized gas storage tank, controlling a valve to enable carrier gas to enter an adsorption column in a suspended mode after 1min, starting a vacuum pump for 3min to pump all residual gas in the adsorption column into the gas storage tank, stopping the vacuum pump, controlling the valve again to enable the carrier gas to flow through the adsorption column, pushing the gas in the gas storage tank to enter a later-stage chromatographic column, and enabling SO in the gas to enter the adsorption column 2 The gas enters a PDHID detector in the absence of SF 6 Under the condition of gas interference, accurately detecting ultralow concentration SO 2 Gas concentration.
This example uses an adsorbent to remove SO 2 The gas is adsorbed and desorbed, thereby separating SO 2 And SF (sulfur hexafluoride) 6 Complete separation of SO 2 Rear and SF 6 Enters a chromatographic column to avoid the detection of SO by a PDHID detector 2 When there is a small amount of SF 6 Thereby avoiding the detection of SO by the PDHID detector 2 When there is a small amount of SF 6 Gas, reducing detection sensitivity and accuracy.
Example 2
For embodiment 1, the detection method is provided in this embodiment, specifically as follows:
step 1, vacuumizing; opening the vacuum pump 14, opening the second electromagnetic valve 13, the third electromagnetic valve 15, the sixth electromagnetic valve 19, the seventh electromagnetic valve 20 and the eleventh electromagnetic valve 28, closing other electromagnetic valves, vacuumizing to a set value, displaying 67Pa by a general vacuum gauge, closing the vacuum pump 14, and closing all the electromagnetic valves;
step 2, purging; the carrier gas (high-purity helium) enters the device of the embodiment 1 from the carrier gas inlet 9, the first electromagnetic valve 10 and the tenth electromagnetic valve 27 are opened, one path of the carrier gas flows to the six-way valve carrier gas inlet 2 to purge the six-way valve 7 (the purging function is to remove the interference of residual gas before, and the following is the same), and the gas after purging is directly discharged; the other path flows to the PDHID detector 24 to purge the PDHID detector 24, the purged gas is discharged to the outside from a detection gas outlet 26 of the PDHID detector 24, and a tenth electromagnetic valve 27 is closed after the purging is finished;
sample gas (containing SO) 2 SF of impurities 6 Gas) enters the six-way valve 7 from the sample gas inlet 6, and at the moment, the six-way valve 7 communicates the sample gas inlet 6 with the sample gas outlet 5 through the cut valve, and the sample gas is discharged to the outside from the sample gas outlet 5, so that the purging of the sample gas pipeline is realized.
Step 3, after purging, the six-way valve 7 is used for communicating the sample gas inlet 6 with the quantitative ring inlet 1 through a cut valve, the sample gas enters the quantitative ring 8, after a certain volume of gas is quantitatively collected, the six-way valve 7 is used for sequentially connecting the carrier gas inlet 2, the quantitative ring inlet 1, the quantitative ring outlet 4 and the carrier gas outlet 3 through the cut valve, and the carrier gas brings the sample gas in the quantitative ring into the subsequent adsorption column 12;
step 4, after the carrier gas containing the sample gas enters the adsorption column 12, all electromagnetic valves are closed at the moment, the gas is stored in the adsorption column 12, and the mixture is kept stand for a set period of time (generally about 2 min) until SO is reached 2 After the gas is fully adsorbed, the third solenoid valve 15, the seventh solenoid valve 20 and the ninth solenoid valve 22 are opened at this time, and only helium and SF are contained 6 The gas enters the post-stage chromatographic column 23, is separated by the chromatographic column, enters the post-stage PDHID detector 24, and is discharged to the outside from the detection gas outlet 26 after detection and analysis;
step 5. After the third solenoid valve 15 is opened for a set period of time, typically 3 minutes, SF in the adsorption column 12 6 The gas is completely pushed out by the carrier gas and enters the chromatographic column 23, at the moment, the third electromagnetic valve 15 and the seventh electromagnetic valve 20 are closed, the six-way valve 7 disconnects the connection between the carrier gas inlet 2 and the dosing ring 8 through the cut valve, and the carrier gas enters the carrier gas inlet 2 and is directly discharged; at this time, the eighth solenoid valve 21 is opened, and the carrier gas continues to enter the chromatographic column 23; then, the heating rod in the adsorption column 12 is started to heat the kdhf-03 type molecular sieve to 100 ℃, the temperature sensor 11 detects the temperature in the adsorption column, the second electromagnetic valve 13 and the fifth electromagnetic valve 17 are opened when the temperature reaches 100 ℃, the vacuum pump 14 is started, and desorbed SO is removed 2 Pumping into a gas storage tank 18, vacuumizing for a set period of time, and adsorbing all SO in the column 12 2 The gas is pumped to the gas storage tank 18, at the moment, the vacuum pump 14 is closed, the second electromagnetic valve 13, the seventh electromagnetic valve 20 and the eighth electromagnetic valve 21 are closed, the third electromagnetic valve 15, the fourth electromagnetic valve 16, the fifth electromagnetic valve 17 and the sixth electromagnetic valve 19 are opened, the six-way valve 7 is used for communicating the carrier gas inlet 2 with the carrier gas outlet 3, and the carrier gas continuously pushes SO in the gas storage tank 18 2 The gas enters a post chromatographic column 23, passes through a PDHID detector 24, is discharged to the outside from a detected gas outlet 26 after detection and analysis, and waits for SO to appear 2 And after the detection result, closing all electromagnetic valves, stopping air inlet, and ending the detection process.
The above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (9)
1. Be applicable to SF 6 The helium ion gas chromatograph for detecting decomposition products is characterized by comprising a six-way valve (7), a quantitative ring (8), an adsorption column (12), a vacuum pump (14), a gas storage tank (18), a chromatographic column (23), a PDHID detector (24) and first to eleventh electromagnetic valves;
the carrier gas inlet (9) is communicated with the carrier gas inlet (2) of the six-way valve, the carrier gas outlet (3) of the six-way valve is communicated with the inlet of the adsorption column, and the outlet of the adsorption column (12) is communicated with the inlet of the chromatographic column (23); the outlet of the chromatographic column (23) is communicated with the inlet of a PDHID detector (24); the carrier gas inlet (9) is communicated with an inlet of a PDHID detector (24);
a first electromagnetic valve (10) is connected in series between the carrier gas inlet (9) and the carrier gas inlet (2) of the six-way valve; a tenth electromagnetic valve (27) is connected in series between the carrier gas inlet (9) and the PDHID detector (24); a third electromagnetic valve (15), a seventh electromagnetic valve (20) and a ninth electromagnetic valve (22) are sequentially connected in series between the adsorption column (12) and the chromatographic column (23); the upstream of the ninth electromagnetic valve (22) is connected with the upstream of the tenth electromagnetic valve (27) in series through an eighth electromagnetic valve (21); a second electromagnetic valve (13), a vacuum pump (14), a fifth electromagnetic valve (17), an air storage tank (18) and a sixth electromagnetic valve (19) are connected in series between the outlet of the adsorption column (12) and the upstream of the ninth electromagnetic valve (22) in sequence; a fourth electromagnetic valve (16) is connected in series between the downstream of the third electromagnetic valve (15) and the outlet of the vacuum pump (14);
introducing the sample gas in the quantitative ring (8) into a later stage adsorption column (12) through carrier gas, wherein the adsorption column (12) contains enough kdhf-03 type molecular sieve, and standing the sample gas and the carrier gas in the adsorption column for a set time, and then, carrying out SO 2 The gas is completely absorbed, and the carrier gas is reused to absorb the gas and only contains helium and SF 6 The gas is purged to a post chromatographic column (23) for separation, a heating rod in an adsorption column (12) is started after a set time period, the molecular sieve is heated to 100 ℃ for desorption, and the desorbed SO is desorbed by carrier gas 2 The gas is led into a small gas storage tank (18), after a set time length, a valve is controlled to enable carrier gas to enter an adsorption column (12) in a suspended mode, a vacuum pump (14) is started to pump all residual gas in the adsorption column (12) into the gas storage tank (18), then the vacuum pump (14) is stopped, the valve is controlled again to enable the carrier gas to flow through the adsorption column (12), the gas in the gas storage tank (18) is pushed to enter a later chromatographic column (23), and SO in the gas 2 The gas enters a PDHID detector (24), in the absence of SF 6 Under the condition of gas interference, accurately detecting ultralow concentration SO 2 Gas concentration.
2. The method according to claim 1Be applicable to SF 6 The helium ion gas chromatograph for detecting the decomposition products is characterized in that a check valve (25) is connected in series on the exhaust pipe of the PDHID detector (24).
3. A method according to claim 1 or 2, suitable for SF 6 The helium ion gas chromatograph for detecting decomposition products is characterized in that an eleventh electromagnetic valve (28) is arranged on an exhaust pipeline of the vacuum pump (14).
4. A method according to claim 1 or 2, suitable for SF 6 Helium ion gas chromatograph for detection of decomposition products, characterized in that the adsorption column (12) comprises a molecular sieve (122) and a heating rod (121), the heating rod (121) heating the molecular sieve (122).
5. A method according to claim 1, suitable for SF 6 The helium ion gas chromatograph for detecting the decomposition products is characterized by comprising the following steps:
(1) Vacuumizing;
(2) Purging;
(3) After purging, the six-way valve (7) is used for communicating the sample gas inlet (6) with the quantitative ring inlet 1 through the cut valve, the sample gas enters the quantitative ring (8), after a certain volume of gas is quantitatively collected, the six-way valve (7) is used for sequentially connecting the carrier gas inlet (2), the quantitative ring inlet (1), the quantitative ring outlet (4) and the carrier gas outlet (3) through the cut valve, and the carrier gas brings the sample gas in the quantitative ring into the later-stage adsorption column (12);
(4) After the carrier gas containing the sample gas enters the adsorption column (12), all electromagnetic valves are closed at the moment, the gas is stored in the adsorption column (12), and the carrier gas is kept stand for a set period of time until SO 2 After the gas is fully adsorbed, the third electromagnetic valve (15), the seventh electromagnetic valve (20) and the ninth electromagnetic valve (22) are opened at the moment, and only helium and SF are contained 6 The gas enters a post-stage chromatographic column (23), is separated by the chromatographic column, enters a post-stage PDHID detector (24), and is discharged to the outside from a detection gas outlet (26) after detection and analysis;
(5) After the third electromagnetic valve (15) is opened for a set period of time, SF in the adsorption column (12) 6 The gas is completely pushed out by the carrier gas and enters the chromatographic column (23), at the moment, the third electromagnetic valve (15) and the seventh electromagnetic valve (20) are closed, the six-way valve (7) disconnects the carrier gas inlet (2) from the quantitative ring (8) through the cut valve, and the carrier gas enters the carrier gas inlet (2) to be directly discharged; the eighth electromagnetic valve (21) is opened at the moment, and the carrier gas continuously enters the chromatographic column (23); then, the heating rod in the adsorption column (12) is started to heat to a set temperature, then the second electromagnetic valve (13) and the fifth electromagnetic valve (17) are opened, the vacuum pump (14) is started, and desorbed SO is obtained 2 Pumping into a gas storage tank (18), vacuumizing for a set period of time, and adsorbing all SO in the column (12) 2 The gas is pumped to a gas storage tank (18), at the moment, a vacuum pump (14) is closed, a second electromagnetic valve (13), a seventh electromagnetic valve (20) and an eighth electromagnetic valve (21) are closed, a third electromagnetic valve (15), a fourth electromagnetic valve (16), a fifth electromagnetic valve (17) and a sixth electromagnetic valve (19) are opened, a six-way valve (7) is used for communicating a carrier gas inlet (2) with a carrier gas outlet (3), and the carrier gas continuously pushes SO in the gas storage tank (18) 2 The gas enters a post chromatographic column (23), passes through a PDHID detector (24), is discharged to the outside from a detected gas outlet (26) after detection and analysis, and waits for SO to appear 2 And after the detection result, closing all electromagnetic valves, stopping air inlet, and ending the detection process.
6. A method according to claim 5, suitable for SF 6 The helium ion gas chromatograph for detecting the decomposition products is characterized in that the specific method for vacuumizing in the step (1) comprises the following steps: the vacuum pump (14) is opened, the second electromagnetic valve (13), the third electromagnetic valve (15), the sixth electromagnetic valve (19), the seventh electromagnetic valve (20) and the eleventh electromagnetic valve (28) are opened, the other electromagnetic valves are closed, vacuum pumping is carried out to a set value, then the vacuum pump (14) is closed, and all the electromagnetic valves are closed.
7. A method according to claim 5, suitable for SF 6 The helium ion gas chromatograph for detecting the decomposition products is characterized in that the specific purging method in the step (2) is as follows: the carrier gas enters from the carrier gas inlet (9), the first electromagnetic valve (10) and the tenth electromagnetic valve (27) are opened, and one path of carrier gas flows to the carrier gas inlet (2) of the six-way valve to purge the six-way valve (7)The swept gas is directly discharged; the other path flows to the PDHID detector (24), the PDHID detector (24) is purged, the purged gas is discharged to the outside from a detection gas outlet (26) of the PDHID detector (24), and a tenth electromagnetic valve (27) is closed after the purging is finished.
8. A method according to claim 7 suitable for SF 6 Helium ion gas chromatograph that decomposition product detected, its characterized in that sweeps still includes the sweep of sample gas line, specifically: sample gas enters the six-way valve (7) from the sample gas inlet (6), at the moment, the six-way valve (7) is communicated with the sample gas inlet (6) and the sample gas outlet (5) through the cut valve, and the sample gas is discharged to the outside from the sample gas outlet (5), so that the purging of the sample gas pipeline is realized.
9. A method according to claim 5, suitable for SF 6 Helium ion gas chromatograph for detection of decomposition products, characterized in that in step (5), the heating rod heats the kdhf-03 type molecular sieve in the adsorption column (12) to 100 ℃.
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