CN203672843U - Heliumion chromatograph for analyzing SF6 (sulfur hexafluoride) decomposition products - Google Patents
Heliumion chromatograph for analyzing SF6 (sulfur hexafluoride) decomposition products Download PDFInfo
- Publication number
- CN203672843U CN203672843U CN201320717445.2U CN201320717445U CN203672843U CN 203672843 U CN203672843 U CN 203672843U CN 201320717445 U CN201320717445 U CN 201320717445U CN 203672843 U CN203672843 U CN 203672843U
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- China
- Prior art keywords
- valve
- column
- porapak
- pdd
- analyzing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- 238000000354 decomposition reaction Methods 0.000 title claims abstract description 25
- 229910018503 SF6 Inorganic materials 0.000 title abstract description 6
- SFZCNBIFKDRMGX-UHFFFAOYSA-N sulfur hexafluoride Chemical compound FS(F)(F)(F)(F)F SFZCNBIFKDRMGX-UHFFFAOYSA-N 0.000 title abstract description 6
- 229960000909 sulfur hexafluoride Drugs 0.000 title abstract description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000000741 silica gel Substances 0.000 claims abstract description 13
- 229910002027 silica gel Inorganic materials 0.000 claims abstract description 13
- 239000001307 helium Substances 0.000 claims description 17
- 229910052734 helium Inorganic materials 0.000 claims description 17
- 229960001866 silicon dioxide Drugs 0.000 claims description 12
- 229910001220 stainless steel Inorganic materials 0.000 claims description 6
- 239000010935 stainless steel Substances 0.000 claims description 6
- 238000000926 separation method Methods 0.000 description 10
- 239000007789 gas Substances 0.000 description 7
- 239000012535 impurity Substances 0.000 description 6
- 239000002245 particle Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 239000005864 Sulphur Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 2
- 230000008878 coupling Effects 0.000 description 2
- 238000010168 coupling process Methods 0.000 description 2
- 238000005859 coupling reaction Methods 0.000 description 2
- VJHINFRRDQUWOJ-UHFFFAOYSA-N dioctyl sebacate Chemical compound CCCCC(CC)COC(=O)CCCCCCCCC(=O)OCC(CC)CCCC VJHINFRRDQUWOJ-UHFFFAOYSA-N 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 230000007257 malfunction Effects 0.000 description 2
- 238000004445 quantitative analysis Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminium flouride Chemical compound F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 description 1
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- 239000012491 analyte Substances 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008033 biological extinction Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 238000010892 electric spark Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 125000000475 sulfinyl group Chemical group [*:2]S([*:1])=O 0.000 description 1
- 125000000472 sulfonyl group Chemical group *S(*)(=O)=O 0.000 description 1
- 230000009967 tasteless effect Effects 0.000 description 1
- TXEYQDLBPFQVAA-UHFFFAOYSA-N tetrafluoromethane Chemical compound FC(F)(F)F TXEYQDLBPFQVAA-UHFFFAOYSA-N 0.000 description 1
- NXHILIPIEUBEPD-UHFFFAOYSA-H tungsten hexafluoride Chemical compound F[W](F)(F)(F)(F)F NXHILIPIEUBEPD-UHFFFAOYSA-H 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
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- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The utility model discloses a heliumion chromatograph for analyzing SF6 (sulfur hexafluoride) decomposition products. The heliumion chromatographcomprises four chromatographic columns, namely, a silica gel column, a first Porapak Q column, a second Porapak Q column and a Gasprocapillary column; the heliumion chromatograph further comprises four valves which correspond to the four chromatographic columns and include a first valve, a second valve, a third valve and a fourth valve, and the four chromatographic columns are connected through the four valves; the heliumion chromatograph further comprises a first PDD (pulsed discharge detector) and a second PDD, the first PDD is connected with the third valve, and the second PDD is connected with the fourth valve. According to the heliumion chromatograph, internal operation conditions of SF6 gas insulated equipment can be judged accurately, so that the safe operation of electrical equipment is guaranteed.
Description
Technical field
The utility model relates to chromatograph, particularly relates to a kind of for analyzing SF
6the helium ion chromatograph of decomposition product.
Background technology
Sulfur hexafluoride (SF
6) be at normal temperatures and pressures a kind of colourless, tasteless, nontoxic, do not fire, the forming gas of chemical property stabilizer pole.SF
6molecule be the symmetrical structure of single sulphur polyfluoro, there is extremely strong electronegativity, give its good electrical isolation and arc extinction performance.At present, SF
6as insulating medium of new generation, be widely used in high pressure, the electric equipment of UHV (ultra-high voltage).Fill SF
6electrical equipment floor area few, running noises is little, without fire hazard, has greatly improved the safe reliability of electric equipment operation.
SF
6gas, under the effect of overheated, electric arc, electric spark and corona discharge, can decompose, its decomposition product also can with equipment in micro-moisture, electrode and solid insulating material react, its product more complicated, has gaseous impurities, as carbon tetrafluoride (CF
4), fluoridize sulfonyl (SO
2f
2), fluoridize thionyl (SOF
2), sulphuric dioxide (SO
2), ten fluorine one are oxidized two sulphur (S
2oF
10) etc., also have some solid impurities, as aluminum fluoride (AlF
3), tungsten fluoride (WF
6) etc., specifically decomposition approach sees the following form.
For operating electrical equipment, judge its device interior running status difficulty relatively, by analyzing and testing SF
6the decomposition product of gas is to judge SF
6strong means of air insulating device internal operation situation.In recent years, Guangdong Province is by detecting SF
6cF in gas
4and SO
2content Deng decomposition product has successfully judged a lot of electrical equipment malfunctions.According to research experience and real work in the past, pass through SF
6the decomposition product SO of gas
2f
2, SOF
2, S
2oF
10, CS
2, the decomposition product such as SCO can effectively judge SF
6air insulating device internal operation situation, meanwhile, passes through H
2, O
2, N
2, CO, CH
4, CO
2, C
2f
6content Deng magazine also can effectively judge SF
6air insulating device internal operation situation, the proposition of this method is strong means that successfully judge electrical equipment malfunction.
Traditional colour spectrometer adopts Gaspro capillary column single-column to come SF
6decomposition product separates and tests, and utilizes TCD and FDP series winding detecting device to SF
6decomposition product is analyzed, not only can Accurate Determining CF
4, C
2f
6, C
3f
8, C
4f
10, SOF
2deng impurity, can also Accurate Determining SO
2f
2, S
2oF
10deng impurity.But rely on single-column to separate and can not effectively analyze H
2, O
2, N
2, CO, CH
4, CO
2, COS, H
2s, SOF
2, CS
2deng compound, and that these compounds judge between right and wrong to the running status of inside electric appliance is normal important.Utilize the detecting device of TCD-FPD series connection also to have shortcoming, TCD sensitivity is low, detects limit for height, can not be used for detecting the decomposition product of low content; FPD detecting device, because it is not linear detector, easily causes error larger quantitatively time, quantitatively inaccurate.
Utility model content
Based on this, be necessary for the problems referred to above, provide a kind of for analyzing SF
6the helium ion chromatograph of decomposition product.
One is used for analyzing SF
6the helium ion chromatograph of decomposition product, is provided with four root chromatogram columns, wherein has a silicagel column, a Porapak Q post, a 2nd Porapak Q post and a Gaspro capillary column;
Also be provided with four valves including first valve, second valve, three valve, four valve corresponding with above-mentioned four root chromatogram columns, described four root chromatogram columns connect by four valves, a wherein said Porapak Q post is connected with described the first valve, described the 2nd Porapak Q post and described the first valve, the 3rd valve interconnect, described silicagel column and described the first valve, the 3rd valve interconnect, and described Gaspro capillary column and described second valve, the 4th valve interconnect;
Also be provided with a PDD detecting device (helium ion detector) and the 2nd PDD detecting device (helium ion detector), wherein, a described PDD detecting device is connected with described the 3rd valve, and described the 2nd PDD detecting device is connected with described the 4th valve.The utility model is connected and can be realized the separation between different component by multicolumn, can realize the switching of sample in different chromatographic columns and different valve, utilizes the characteristic of different chromatographic columns to realize effective separation of various impurity in sample.Acting as of above-mentioned four chromatographic column couplings carried out component separation to sample, and cutting of components separation control is carried out in acting as of above-mentioned four valves; Above-mentioned two PDD detecting devices detect the sample after separating respectively, and wherein a PDD detecting device is used for detecting H
2, O
2, N
2, CH
4, CF
4, CO, CO
2, C
2f
6, the 2nd PDD detecting device is used for detecting C
2h
2, COS, C
2, H
2s, SO
2f
2, C
3f
8, C
3, CS
2, SO
2, S
2oF
10.
In an embodiment, described silicagel column is the stainless steel column of long 3m, internal diameter 3mm therein, the silica gel of what in-built particle diameter was 0.30mm～0.60mm scribble Plexol 201.Above-mentioned silicagel column can be realized H
2, O
2and N
2effective separation.
In an embodiment, a described Porapak Q post and the 2nd Porapak Q post are the stainless-steel tube of long 2m, internal diameter 3mm, the Porapak Q that in-built particle diameter is 0.18mm～0.25mm therein.Above-mentioned Porapak Q post can be realized CF
4, C
2f
6, C
3f
8effective separation.
In an embodiment, described Gaspro capillary column is long 60m therein, the GasPro capillary chromatographic column of internal diameter 0.32 μ m.Above-mentioned Gaspro capillary column can be realized C
2h
2, COS, C
2, H
2s, SO
2f
2, C
3f
8, C
3, CS
2, SO
2and S
2oF
10separation.
The utility model compared to advantage and the beneficial effect of prior art is:
By multidigit inventor years of researches and a large amount of experiments, invent the utility model helium ion chromatograph, said apparatus is connected and can be realized the separation between different component by multicolumn,, can accurately detect the SF that traditional colour spectrometer can not accurately detect simultaneously
6decomposition product, as H
2, O
2, N
2, CO, CH
4, CO
2, COS, H
2s, SOF
2, CS
2deng compound, by comprehensive and accurate to SF
6decomposition product is analyzed, thereby accurately judges SF
6air insulating device internal operation situation, ensures electrical equipment safe operation.
Accompanying drawing explanation
Fig. 1 is that the utility model is for analyzing SF
6valve in the helium ion chromatograph of decomposition product and post connection layout (4 valves are closed condition), description of reference numerals: 100: the Porapak Q posts; 200: silicagel column; 300: the two Porapak Q posts; 400:Gaspro capillary column; 500: the first valves; 600: second valve; 700: the three valves; 800: the four valves; 900: quantity tube; 110: injection port; 120: the PDD detecting devices; 130: the two PDD detecting devices;
Fig. 2 is that the utility model is for analyzing SF
6valve in the helium ion chromatograph of decomposition product and post connection layout (4 valves are opening);
Fig. 3 is the spectrogram of a PDD detecting device gained in embodiment 1;
Fig. 4 is the spectrogram of the 2nd PDD detecting device gained in embodiment 1;
Fig. 5 analyzes gained chromatogram by traditional colour spectrometer.
Embodiment
Embodiment 1
One is used for analyzing SF
6the helium ion chromatograph of decomposition product, be provided with four root chromatogram columns, wherein there is a long 3m of silicagel column 200(, the stainless steel column of internal diameter 3mm, in-built particle diameter is the silica gel that scribbles Plexol 201 of 0.30mm～0.60mm), a the one Porapak Q post 100, the 2nd Porapak Q post 300(the one Porapak Q post 100 and the 2nd Porapak Q post 300 are long 2m, the stainless-steel tube of internal diameter 3mm, in-built particle diameter is the Porapak Q of 0.18mm～0.25mm) and a long 60m of Gaspro capillary column 400(, the GasPro capillary chromatographic column of internal diameter 0.32 μ m), and be provided with comprise first valve 500 corresponding with above-mentioned four root chromatogram columns, second valve 600, the 3rd valve 700, the 4th valve 800 is at four interior valves, described four root chromatogram columns connect (second valve 600 by four valves, the 3rd valve 700, the 4th valve 800 is six-way valve, the first valve 500 is ten-way valve), wherein a Porapak Q post 100 is connected with the first valve 500, the 2nd Porapak Q post 300 and the first valve 500, the 3rd valve 700 interconnect, silicagel column 200 and the first valve 500, the 3rd valve 700 interconnect, and Gaspro capillary column 400 interconnects with second valve 600, the 4th valve 800, acting as of above-mentioned four chromatographic column couplings carried out component separation to sample, and cutting of components separation control is carried out in acting as of above-mentioned four valves,
Also be provided with a PDD detecting device (helium ion detector) 120 and the 2nd PDD detecting device (helium ion detector) 130, wherein, a PDD detecting device 120 is connected with the 3rd valve 700, and the 2nd PDD detecting device 130 is connected with the 4th valve 800.Above-mentioned two PDD detecting devices detect analysis to the sample after separating respectively, and wherein a PDD detecting device 120 is used for detecting H
2, O
2, N
2, CH
4, CF
4, CO, CO
2, C
2f
6, the 2nd PDD detecting device 130 is used for detecting C
2h
2, COS, C
2, H
2s, SO
2f
2, C
3f
8, C
3, CS
2, SO
2and S
2oF
10.
Be the initial state of four valves as shown in fig. 1, be closed condition; Opening refers to that the connecting line in valve changes completely, and becoming of being originally communicated with is not communicated with, originally disconnected connection, the pipeline constant (as shown in Figure 2) of outside of becoming.Four valves at the changeover program of analytic process are: the initial state of four valves is closes, and wherein the first valve 500 is: 0min, and the first valve 500 is opened; 2min, the first valve 500 cuts out; Second valve 600 is: 0min, and second valve 600 is opened; 4.2min, second valve 600 is closed; The 3rd valve 700 is: 4.4min, and the 3rd valve 700 is opened; 16.7min, the 3rd valve 700 cuts out; The 4th valve 800 is: 0min, and the 4th valve 800 is opened; 4.5min, the 4th valve 800 cuts out.Wherein, when the first valve 500 closed condition, can realize sample and rinse entering quantity tube 900, in preparing sample introduction state, when opening, sample, from injection port 110 sample introductions, is progressively delivered to each chromatographic column by carrier gas and is analyzed; The open and close of second valve 600 can realize sample and whether enter Gaspro capillary column 400 and separate; The open and close of the 3rd valve 700 can determine whether the sample after chromatographic column separates enters a PDD detecting device 120 and carry out analyzing and testing; The 4th valve 800 can determine whether the sample after Gaspro capillary column 400 separates enters the 2nd PDD detecting device 130 and carry out analyzing and testing.
The parameter of utilizing the utility model to carry out analyte detection process (two PDD detecting devices are following parameter) is: carrier gas: helium, and purity >=99.999%, output pressure is 0.5Mpa, flow velocity 50nl/min; Drive gas: air/nitrogen, driving gas output pressure is 0.3Mpa, flow velocity 70nl/min, sample introduction pressure: 0.05Mpa; Column temperature (four chromatographic columns are following condition) condition is: initial 40 ℃ keep 8min to be then raised to 180 ℃ of maintenances 5 minutes with 10 ℃/min.
Fig. 3 and Fig. 4 are the chromatogram of the present embodiment gained, and wherein Fig. 3 is PDD detecting device 120 gained chromatograms, and peak sequence is: H
2, O
2, N
2, CO, CF
4, CH
4, CO
2, C
2f
6; And use traditional chromatograph (as shown in Figure 5) can not effectively separate H
2, O
2and N
2, can not accurate quantitative analysis Analysis for CO, CH
4, CO
2and C
2f
6.Fig. 4 is the 2nd PDD detecting device 130 gained chromatograms.Inventor's discovery of the present utility model, peak sequence is: C
2h
2, COS, C
2, H
2s, SO
2f
2, C
3f
8, C
3, CS
2, SO
2, S
2oF
10, these impurity (SF
6decomposition product) in have not simultaneously exist, therefore can not provide on individual chromatogram; And use traditional chromatograph (as shown in Figure 5) can not effectively separate SO
2f
2and C
3f
8, can not analyze C by accurate quantitative analysis
2h
2, COS, C
2, C
3, CS
2and S
2oF
10.
The above embodiment has only expressed several embodiment of the present utility model, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to the utility model the scope of the claims.It should be pointed out that for the person of ordinary skill of the art, without departing from the concept of the premise utility, can also make some distortion and improvement, these all belong to protection domain of the present utility model.Therefore, the protection domain of the utility model patent should be as the criterion with claims.
Claims (4)
1. one kind for analyzing SF
6the helium ion chromatograph of decomposition product, is characterized in that, is provided with four root chromatogram columns, wherein has a silicagel column, a Porapak Q post, a 2nd Porapak Q post and a Gaspro capillary column;
Also be provided with four valves including first valve, second valve, three valve, four valve corresponding with above-mentioned four root chromatogram columns, described four root chromatogram columns connect by four valves, a wherein said Porapak Q post is connected with described the first valve, described the 2nd Porapak Q post and described the first valve, the 3rd valve interconnect, described silicagel column and described the first valve, the 3rd valve interconnect, and described Gaspro capillary column and described second valve, the 4th valve interconnect;
Also be provided with a PDD detecting device and the 2nd PDD detecting device, wherein, a described PDD detecting device is connected with described the 3rd valve, and described the 2nd PDD detecting device is connected with described the 4th valve.
2. according to claim 1 for analyzing SF
6the helium ion chromatograph of decomposition product, is characterized in that, described silicagel column is the stainless steel column of long 3m, internal diameter 3mm.
3. according to claim 1 for analyzing SF
6the helium ion chromatograph of decomposition product, is characterized in that, a described Porapak Q post and the 2nd Porapak Q post are the stainless-steel tube of long 2m, internal diameter 3mm.
4. according to claim 1 for analyzing SF
6the helium ion chromatograph of decomposition product, is characterized in that, described Gaspro capillary column is long 60m, the GasPro capillary chromatographic column of internal diameter 0.32 μ m.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201320717445.2U CN203672843U (en) | 2013-11-13 | 2013-11-13 | Heliumion chromatograph for analyzing SF6 (sulfur hexafluoride) decomposition products |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201320717445.2U CN203672843U (en) | 2013-11-13 | 2013-11-13 | Heliumion chromatograph for analyzing SF6 (sulfur hexafluoride) decomposition products |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN203672843U true CN203672843U (en) | 2014-06-25 |
Family
ID=50969124
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201320717445.2U Expired - Lifetime CN203672843U (en) | 2013-11-13 | 2013-11-13 | Heliumion chromatograph for analyzing SF6 (sulfur hexafluoride) decomposition products |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN203672843U (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104155402A (en) * | 2014-08-27 | 2014-11-19 | 上海华爱色谱分析技术有限公司 | Helium ionization gas chromatography system for analyzing decomposition products of SF6 |
-
2013
- 2013-11-13 CN CN201320717445.2U patent/CN203672843U/en not_active Expired - Lifetime
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104155402A (en) * | 2014-08-27 | 2014-11-19 | 上海华爱色谱分析技术有限公司 | Helium ionization gas chromatography system for analyzing decomposition products of SF6 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CX01 | Expiry of patent term | ||
| CX01 | Expiry of patent term |
Granted publication date: 20140625 |