CN103604882B - 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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- CN103604882B CN103604882B CN201310566033.8A CN201310566033A CN103604882B CN 103604882 B CN103604882 B CN 103604882B CN 201310566033 A CN201310566033 A CN 201310566033A CN 103604882 B CN103604882 B CN 103604882B
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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 analysis detection 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 excellent electrical isolation and arc extinction performance.At present, SF
6as the insulating medium of a new generation, be widely used in high pressure, extra-high voltage electrical equipment.Fill SF
6electrical equipment floor area few, running noises is little, without fire hazard, drastically increases the safe reliability of electric equipment operation.
SF
6gas is under the effect of overheated, electric arc, electric spark and corona discharge, and can decompose, its decomposition product also can react with the micro-moisture in equipment, electrode and solid insulating material, and 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., concrete decomposition approach sees the following form.
For operating electrical equipment, judging its device interior running status relative difficulty, detecting SF by analyzing
6the decomposition product of gas judges 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 malfunction.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 effectively can 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 effectively can judge SF
6air insulating device internal operation situation, the proposition of this method is the strong means successfully judging electrical equipment malfunction.
Traditional colour spectral analysis method adopts Gaspro capillary column single-column to come SF
6decomposition product carries out being separated and testing, and utilizes TCD and FDP to contact detecting device to SF
6decomposition product is analyzed, can not only 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 be separated and effectively can not analyze H
2, O
2, N
2, CO, CH
4, CO
2, COS, H
2s, SOF
2, CS
2deng compound, and the running status of these compounds to inside electric appliance judges between right and wrong often important.The detecting device utilizing TCD-FPD to connect also has shortcoming, and TCD sensitivity is low, detects limit for height, can not be used for detecting the decomposition product of low content; FPD detecting device is not linear detector due to it, easily causes error comparatively large, quantitatively inaccurate when quantitative.
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 accurately can detect the SF that traditional analysis can not accurately detect simultaneously
6decomposition product, by comprehensive and accurate to SF
6decomposition product is analyzed, thus 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 a silicagel column, four root chromatogram column couplings of a Porapak Q post, a 2nd Porapak Q post and a Gaspro capillary column carry out Component seperation to sample, adopt comprise the first valve, the second valve, the 3rd valve, the 4th valve four valves carry out cutting of components and be separated and control, adopt a PDD detecting device and the 2nd PDD detecting device to carry out analytical test respectively to the sample after being separated.
Wherein in some embodiments, described four root chromatogram columns are connected by described four valves, a wherein said Porapak Q post is connected with described first valve, described 2nd Porapak Q post and described first valve, the 3rd valve are interconnected, described silicagel column and described first valve, the 3rd valve are interconnected, and described Gaspro capillary column and described second valve, the 4th valve are interconnected;
A described PDD detecting device is connected with described 3rd valve, and described 2nd PDD detecting device is connected with described 4th valve.
The present invention to be connected the separation that can realize between different component by multicolumn, can realize the switching of sample in different chromatographic column and different valve, utilize the characteristic of different chromatographic column to realize various impurity (SF in sample
6decomposition product) effective separation.
Wherein in an embodiment, 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 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.
Wherein in some embodiments, described four valves at the changeover program of analytic process are: the initial state of four valves is closedown, and wherein the first valve is: 0min, and the first valve is opened; 2min, the first valve cuts out; Second valve is: 0min, and the second valve is opened; 4.2min, the second valve cuts out; 3rd valve is: 4.4min, and the 3rd valve is opened; 16.7min, the 3rd valve cuts out; 4th valve is: 0min, and the 4th valve is opened; 4.5min, the 4th valve cuts out.
Wherein in some embodiments, described column temperature condition is: initial 40 DEG C keep 8min to be then raised to 180 DEG C of maintenances 5 minutes with 10 DEG C/min.
Wherein in some embodiments, analyzing detected parameters is: carrier gas: helium, and purity >=99.999%(is preferably 99.9999%), output pressure is 0.5-0.6Mpa, flow velocity 40-70nl/min; Drive gas: air/nitrogen, drive gas output pressure to be 0.3-0.4Mpa, flow velocity 50-100nl/min, sample introduction pressure: 0.05Mpa.
Wherein in some embodiments, described analysis detected parameters is: carrier gas: helium, purity >=99.999%, and output pressure is 0.5Mpa, flow velocity 50nl/min; Drive gas: air/nitrogen, drive gas output pressure to be 0.3Mpa, flow velocity 70nl/min, sample introduction pressure: 0.05Mpa.
Wherein in an embodiment, described silicagel column is the stainless steel column of long 3m, internal diameter 3mm, and in-built particle diameter is the silica gel scribbling Plexol 201 of 0.30mm ~ 0.60mm.Above-mentioned silicagel column can realize H
2, O
2and N
2effective separation.
Wherein in some embodiments, a described Porapak Q post and the 2nd Porapak Q post are the stainless-steel tube of long 2m, internal diameter 3mm, and in-built particle diameter is Porapak Q(high molecular polymer of 0.18mm ~ 0.25mm).Above-mentioned Porapak Q post can realize CF
4, C
2f
6, C
3f
8effective separation.
Wherein in some embodiments, described Gaspro capillary column is long 60m, the GasPro capillary chromatographic column of internal diameter 0.32 μm.Above-mentioned Gaspro capillary column can realize 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 the advantage of prior art and beneficial effect is:
The present invention by multidigit inventor years of researches and a large amount of experiments, determines optimized parameter and the combination thereof of analytic process, and connect the separation that can realize between different component by multicolumn, can the accurate detection traditional analysis SF that 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, thus 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 one Porapak Q posts; 200: silicagel column; 300: the two Porapak Q posts; 400:Gaspro capillary column; 500: the first valves; 600: the second valves; 700: the three valves; 800: the four valves; 900: quantity tube; 110: injection port; 120: the one 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 scribbling Plexol 201 of 0.30mm ~ 0.60mm), an one Porapak Q post 100, 2nd Porapak Q post 300(an 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 μm) four chromatographic column couplings Component seperation is carried out to sample, employing comprises the first valve 500, second valve 600, 3rd valve 700, 4th valve 800 carries out cutting of components at interior four valves and is separated control, a PDD detecting device (helium ion detector) 120 and the 2nd PDD detecting device (helium ion detector) 130 is adopted to carry out analytical test respectively to the sample after being separated.As shown in Figure 1, described four root chromatogram columns are undertaken connecting that (the second valve 600, the 3rd valve 700, the 4th valve 800 are six-way valve by four valves; First valve 500 is ten-way valve), wherein a Porapak Q post 100 is connected with the first valve 500,2nd Porapak Q post 300 and the first valve 500, the 3rd valve 700 are interconnected, silicagel column 200 and the first valve 500, the 3rd valve 700 are interconnected, and Gaspro capillary column 400 and the second valve 600, the 4th valve 800 are interconnected;
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 carry out detection to the sample after separation respectively and analyze, 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 is changed completely, and what be originally communicated with becomes and be not communicated with, and originally disconnectedly becomes connection, outside pipeline constant (as shown in Figure 2).Four valves at the changeover program of analytic process are: the initial state of four valves is closedown, 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 the second valve 600 is opened; 4.2min, the second valve 600 cuts out; 3rd valve 700 is: 4.4min, and the 3rd valve 700 is opened; 16.7min, the 3rd valve 700 cuts out; 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 entering quantity tube 900 rinses, and be in and prepare sample introduction state, during opening, sample, from injection port 110 sample introduction, is progressively delivered to each chromatographic column by carrier gas and analyzed; The open and close of the second valve 600 can realize sample and whether enter Gaspro capillary column 400 and be separated; The open and close of the 3rd valve 700 then can determine whether the sample after chromatographic column is separated enters a PDD detecting device 120 and carry out analysis detection; 4th valve 800 can determine whether the sample after Gaspro capillary column 400 is separated enters the 2nd PDD detecting device 130 and carry out analysis detection.
(two PDD detecting devices are following parameter) parameter of analytical approach testing process of the present invention is: carrier gas: helium, purity >=99.999%, and output pressure is 0.5Mpa, flow velocity 50nl/min; Drive gas: air/nitrogen, drive gas output pressure to be 0.3Mpa, flow velocity 70nl/min, sample introduction pressure: 0.05Mpa; Column temperature (four chromatographic columns are following condition) condition is: initial 40 DEG C keep 8min to be then raised to 180 DEG C of maintenances 5 minutes with 10 DEG C/min.
Fig. 3 and Fig. 4 is the chromatogram of the present embodiment gained, and wherein Fig. 3 is a PDD detecting device 120 gained chromatogram, 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) effectively can not be separated H
2, O
2and N
2, can not accurate quantitative analysis CO, CH
4, CO
2and C
2f
6.Fig. 4 is the 2nd PDD detecting device 130 gained chromatogram.Inventor finds, 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 do not exist simultaneously, therefore can not to provide on individual chromatogram; And use traditional chromatogram analysis method (as shown in Figure 5) effectively can not be separated SO
2f
2and C
3f
8, can not accurate quantitative analysis C
2h
2, COS, C
2, C
3, CS
2and S
2oF
10.
The above embodiment only have expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but therefore can not 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 (7)
1. a SF
6the helium Ion Chromatographic Method of decomposition product, it is characterized in that, employing comprises a silicagel column, four root chromatogram column couplings of a Porapak Q post, a 2nd Porapak Q post and a Gaspro capillary column carry out Component seperation to sample, adopt comprise the first valve, the second valve, the 3rd valve, the 4th valve four valves carry out cutting of components and be separated and control, adopt a PDD detecting device and the 2nd PDD detecting device to carry out analytical test respectively to the sample after being separated;
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 2nd PDD detecting device is used for detecting C
2h
2, COS, H
2s, SO
2f
2, C
3f
8, CS
2, SO
2, S
2oF
10;
Described four valves at the changeover program of analytic process are: the initial state of four valves is closedown, and wherein the first valve is: 0min, and the first valve is opened; 2min, the first valve cuts out; Second valve is: 0min, and the second valve is opened; 4.2min, the second valve cuts out; 3rd valve is: 4.4min, and the 3rd valve is opened; 16.7min, the 3rd valve cuts out; 4th valve is: 0min, and the 4th valve is opened; 4.5min, the 4th valve cuts out;
Described four root chromatogram columns are connected by described four valves, a wherein said Porapak Q post is connected with described first valve, described 2nd Porapak Q post and described first valve, the 3rd valve are interconnected, described silicagel column and described first valve, the 3rd valve are interconnected, and described Gaspro capillary column and described second valve, the 4th valve are interconnected;
A described PDD detecting device is connected with described 3rd valve, and described 2nd PDD detecting device is connected with described 4th valve.
2. SF according to claim 1
6the helium Ion Chromatographic Method of decomposition product, is characterized in that, column temperature condition is: initial 40 DEG C keep 8min to be then raised to 180 DEG C of maintenances 5 minutes with 10 DEG C/min.
3. SF according to claim 1
6the helium Ion Chromatographic Method of decomposition product, is characterized in that, analyzes detected parameters to be: carrier gas: helium, purity>=99.999%, and output pressure is 0.5-0.6Mpa, flow velocity 40-70nl/min; Drive gas: air/nitrogen, drive gas output pressure to be 0.3-0.4Mpa, flow velocity 50-100nl/min, sample introduction pressure: 0.05Mpa.
4. SF according to claim 3
6the helium Ion Chromatographic Method of decomposition product, is characterized in that, described analysis detected parameters is: carrier gas: helium, purity>=99.999%, and output pressure is 0.5Mpa, flow velocity 50nl/min; Drive gas: air/nitrogen, drive gas output pressure to be 0.3Mpa, flow velocity 70nl/min, sample introduction pressure: 0.05Mpa.
5. 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, and in-built particle diameter is the silica gel scribbling Plexol 201 of 0.30mm ~ 0.60mm.
6. 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, and in-built particle diameter is the Porapak Q of 0.18mm ~ 0.25mm.
7. 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 μm.
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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 |
| 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 |
| CN110726785B (en) * | 2019-10-25 | 2022-07-08 | 陕西师范大学 | 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 |