CN103604882A - Helium ion chromatographic analysis method for SF6 (sulfur hexafluoride) decomposition product - Google Patents
Helium ion chromatographic analysis method for SF6 (sulfur hexafluoride) decomposition product Download PDFInfo
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- CN103604882A CN103604882A CN201310566033.8A CN201310566033A CN103604882A CN 103604882 A CN103604882 A CN 103604882A CN 201310566033 A CN201310566033 A CN 201310566033A CN 103604882 A CN103604882 A CN 103604882A
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Abstract
The invention discloses a helium ion chromatographic analysis method for a SF6 (sulfur hexafluoride) decomposition product. The method comprises the following steps: separating components of a sample by adopting a combination of four chromatographic columns, comprising a silica gel column, a first Porapak Q column, a second Porapak Q column and a Gaspro capillary column; performing component cutting separation and control by adopting for valves comprising a first valve, a second valve, a third valve and a fourth valve, and respectively analyzing and testing the separated sample by adopting a first PDD detector and a second PDD detector. According to the analysis method, the SF6 decomposition products, such as H2, O2, N2, CO, CH4, CO2, COS, H2S, SOF2, CS2 and other compounds, which cannot be accurately detected by a traditional analysis method can be simultaneously and accurately detected, and the SF6 decomposition products are comprehensively and accurately analyzed, so that the internal operating conditions of SF6 gas insulated equipment are accurately judged, and the safety operation of electrical equipment is guaranteed.
Description
Technical field
The present invention relates to analyzing and testing field, particularly relate to a kind of SF
6the helium Ion Chromatographic Method 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 oxidation 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 judgement 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 former studies experience and real work, 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 spectral analysis method adopts Gaspro capillary column single-column to come SF
6decomposition product carries out separation and test, 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 separation 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.
Summary of the invention
Based on this, be necessary for the problems referred to above, a kind of SF is provided
6the helium Ion Chromatographic Method of decomposition product, it can accurately detect the SF that traditional analysis can not accurately detect simultaneously
6decomposition product, 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.
A kind of SF
6the helium Ion Chromatographic Method of decomposition product, employing comprises that four root chromatogram column couplings of a silicagel column, a Porapak Q post, a 2nd Porapak Q post and a Gaspro capillary column carry out component separation to sample, employing comprises that four valves of the first valve, second valve, the 3rd valve, the 4th valve carry out the separated control of cutting of components, adopt a PDD detecting device, with the 2nd PDD detecting device, the sample after separated is carried out respectively to analytical test.
Therein in some embodiment, described four root chromatogram columns connect by described 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;
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 present invention 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 various impurity (SF in sample
6decomposition product) effective separation.
In an embodiment, a described PDD detecting device is used for detecting H therein
2, O
2, N
2, CH
4, CF
4, CO, CO
2, C
2f
6; Described 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 some embodiment, described four valves at the changeover program of analytic process are: the initial state of four valves is closes, and wherein the first valve is therein: 0min, and the first valve is opened; 2min, the first valve cuts out; Second valve is: 0min, and second valve is opened; 4.2min, second valve is closed; The 3rd valve is: 4.4min, and the 3rd valve is opened; 16.7min, the 3rd valve cuts out; The 4th valve is: 0min, and the 4th valve is opened; 4.5min, the 4th valve cuts out.
In some embodiment, described column temperature condition is therein: initial 40 ℃ keep 8min then with 10 ℃/min, to be raised to 180 ℃ of maintenances 5 minutes.
In some embodiment, analyzing and testing parameter is: carrier gas therein: helium, purity >=99.999%(preferably 99.9999%), output pressure is 0.5-0.6Mpa, flow velocity 40-70nl/min; Drive gas: air/nitrogen, driving gas output pressure is 0.3-0.4Mpa, flow velocity 50-100nl/min, sample introduction pressure: 0.05Mpa.
In some embodiment, described analyzing and testing parameter is: carrier gas therein: 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.
In an embodiment, described silicagel column is the stainless steel column of long 3m, internal diameter 3mm therein, the silica gel that scribbles Plexol 201 that in-built particle diameter is 0.30mm～0.60mm.Above-mentioned silicagel column can be realized H
2, O
2and N
2effective separation.
In some embodiment, a described Porapak Q post and the 2nd Porapak Q post are the stainless-steel tube of long 2m, internal diameter 3mm therein, Porapak Q(high molecular polymer that in-built particle diameter is 0.18mm～0.25mm).Above-mentioned Porapak Q post can be realized CF
4, C
2f
6, C
3f
8effective separation.
In some 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 present invention compared to advantage and the beneficial effect of prior art is:
The present invention, by multidigit inventor years of researches and a large amount of experiments, has determined optimized parameter and the combination thereof of analytic process, and has been connected and can be realized the separation between different component by multicolumn, can accurately detect the SF that traditional analysis 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 SF of the present invention
6valve in the helium Ion Chromatographic Method of decomposition product in chromatograph used 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 SF of the present invention
6valve in the helium Ion Chromatographic Method of decomposition product in chromatograph used 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 is by traditional colour Spectral Analysis gained chromatogram.
Embodiment
Embodiment 1
A kind of SF
6the helium Ion Chromatographic Method of decomposition product, employing comprises 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) four chromatographic column couplings are carried out component separation to sample, employing comprises the first valve 500, second valve 600, the 3rd valve 700, the 4th valve 800 carries out the separated control of cutting of components at four interior valves, sample after adopting 130 pairs of a PDD detecting device (helium ion detector) 120 and the 2nd PDD detecting devices (helium ion detector) separated carries out respectively analytical test.As shown in Figure 1, described four root chromatogram columns connect by four valves that (second valve 600, the 3rd valve 700, the 4th valve 800 are 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;
The one 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 separation 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
2, 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, during the first valve 500 closed condition, can realize sample and rinse entering quantity tube 900, in preparing sample introduction state, during 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 carry out separation; The open and close of the 3rd valve 700 can determine whether the sample after chromatographic column separation enters a PDD detecting device 120 and carry out analyzing and testing; The 4th valve 800 can determine whether the sample after 400 separation of Gaspro capillary column enters the 2nd PDD detecting device 130 and carry out analyzing and testing.
(two PDD detecting devices are following parameter) parameter of analytical approach testing process of the present invention 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 then with 10 ℃/min, to be raised to 180 ℃ of maintenances 5 minutes.
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 chromatogram analysis method (as shown in Figure 5) can not effective separated 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, 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
6what decomposition product), have does not exist simultaneously, therefore can not provide on individual chromatogram; And use traditional chromatogram analysis method (as shown in Figure 5) can not effective separated 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 invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (10)
1. a SF
6the helium Ion Chromatographic Method of decomposition product, it is characterized in that, employing comprises that four root chromatogram column couplings of a silicagel column, a Porapak Q post, a 2nd Porapak Q post and a Gaspro capillary column carry out component separation to sample, employing comprises that four valves of the first valve, second valve, the 3rd valve, the 4th valve carry out the separated control of cutting of components, adopt a PDD detecting device, with the 2nd PDD detecting device, the sample after separated is carried out respectively to analytical test.
2. SF according to claim 1
6the helium Ion Chromatographic Method of decomposition product, it is characterized in that, described four root chromatogram columns connect by described 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;
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.
3. SF according to claim 1
6the helium Ion Chromatographic Method of decomposition product, is characterized in that, a described PDD detecting device is used for detecting H
2, O
2, N
2, CH
4, CF
4, CO, CO
2, C
2f
6; Described 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.
4. SF according to claim 1
6the helium Ion Chromatographic Method of decomposition product, is characterized in that, described four valves at the changeover program of analytic process are: the initial state of four valves is closes, and wherein the first valve is: 0min, and the first valve is opened; 2min, the first valve cuts out; Second valve is: 0min, and second valve is opened; 4.2min, second valve is closed; The 3rd valve is: 4.4min, and the 3rd valve is opened; 16.7min, the 3rd valve cuts out; The 4th valve is: 0min, and the 4th valve is opened; 4.5min, the 4th valve cuts out.
5. according to the SF described in claim 1-4 any one
6the helium Ion Chromatographic Method of decomposition product, is characterized in that, described column temperature condition is: initial 40 ℃ keep 8min then with 10 ℃/min, to be raised to 180 ℃ of maintenances 5 minutes.
6. according to the SF described in claim 1-4 any one
6the helium Ion Chromatographic Method of decomposition product, is characterized in that, analyzing and testing parameter is: carrier gas: helium, and purity>=99.999%, output pressure is 0.5-0.6Mpa, flow velocity 40-70nl/min; Drive gas: air/nitrogen, driving gas output pressure is 0.3-0.4Mpa, flow velocity 50-100nl/min, sample introduction pressure: 0.05Mpa.
7. SF according to claim 6
6the helium Ion Chromatographic Method of decomposition product, is characterized in that, described analyzing and testing 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.
8. SF according to claim 1
6the helium Ion Chromatographic Method of decomposition product, is characterized in that, described silicagel column is the stainless steel column of long 3m, internal diameter 3mm, the silica gel that scribbles Plexol 201 that in-built particle diameter is 0.30mm～0.60mm.
9. SF according to claim 1
6the helium Ion Chromatographic Method 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, the Porapak Q that in-built particle diameter is 0.18mm～0.25mm.
10. SF according to claim 1
6the helium Ion Chromatographic Method 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.
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| CN109030651A (en) * | 2018-08-09 | 2018-12-18 | 全椒南大光电材料有限公司 | Twin columns separation detecting system and detection method based on heartcut |
| CN109459511A (en) * | 2018-11-14 | 2019-03-12 | 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 | Helium ion detector and subject breaker decomposition product mixed gas separation method |
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| CN104267132A (en) * | 2014-08-26 | 2015-01-07 | 广东电网公司电力科学研究院 | Chromatography method for detecting SF6 decomposition products |
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| CN109975449A (en) * | 2017-12-28 | 2019-07-05 | 内蒙古伊泰煤基新材料研究院有限公司 | The Gas Chromatographic Method of hydrogen sulfide and carbonyl sulfur in a kind of crude synthesis gas |
| CN108896691A (en) * | 2018-08-07 | 2018-11-27 | 朗析仪器（上海）有限公司 | One kind is for detecting SF6The multiple-dimension gas phase chromatographic device of decomposition product full constituent |
| CN109030651A (en) * | 2018-08-09 | 2018-12-18 | 全椒南大光电材料有限公司 | Twin columns separation detecting system and detection method based on heartcut |
| CN109030651B (en) * | 2018-08-09 | 2022-01-28 | 全椒南大光电材料有限公司 | Double-column separation detection system and detection method based on center cutting |
| CN109459511A (en) * | 2018-11-14 | 2019-03-12 | 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 | Helium ion detector and subject breaker decomposition product mixed gas separation method |
| CN110726785A (en) * | 2019-10-25 | 2020-01-24 | 国网陕西省电力公司电力科学研究院 | SF analysis based on GC-Q-ToF-MS6Method for medium trace permanent gas |
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Address after: 510080 Dongfeng East Road, Dongfeng, Guangdong, Guangzhou, Zhejiang Province, No. 8 Patentee after: ELECTRIC POWER RESEARCH INSTITUTE, GUANGDONG POWER GRID CO., LTD. Address before: 510080 Dongfeng East Road, Dongfeng, Guangdong, Guangzhou, Zhejiang Province, No. 8 Patentee before: Electrical Power Research Institute of Guangdong Power Grid Corporation |