CN103616468A - SF (sulfur hexafluoride)6Gas chromatography detection system and method - Google Patents
SF (sulfur hexafluoride)6Gas chromatography detection system and method Download PDFInfo
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- CN103616468A CN103616468A CN201310612969.XA CN201310612969A CN103616468A CN 103616468 A CN103616468 A CN 103616468A CN 201310612969 A CN201310612969 A CN 201310612969A CN 103616468 A CN103616468 A CN 103616468A
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- 238000001514 detection method Methods 0.000 title claims abstract description 79
- 238000000034 method Methods 0.000 title abstract description 27
- SFZCNBIFKDRMGX-UHFFFAOYSA-N sulfur hexafluoride Chemical compound FS(F)(F)(F)(F)F SFZCNBIFKDRMGX-UHFFFAOYSA-N 0.000 title description 5
- 238000004587 chromatography analysis Methods 0.000 title description 2
- 229910018503 SF6 Inorganic materials 0.000 title 1
- 229960000909 sulfur hexafluoride Drugs 0.000 title 1
- 238000004817 gas chromatography Methods 0.000 claims abstract description 59
- 230000004044 response Effects 0.000 claims abstract description 25
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 14
- 239000011593 sulfur Substances 0.000 claims abstract description 14
- 238000005070 sampling Methods 0.000 claims description 74
- 238000012546 transfer Methods 0.000 claims description 18
- 238000010790 dilution Methods 0.000 claims description 10
- 239000012895 dilution Substances 0.000 claims description 10
- 238000004445 quantitative analysis Methods 0.000 claims description 9
- 238000010812 external standard method Methods 0.000 claims description 8
- 238000002438 flame photometric detection Methods 0.000 claims description 7
- 238000004451 qualitative analysis Methods 0.000 claims description 7
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 4
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 3
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 3
- 238000002485 combustion reaction Methods 0.000 claims description 3
- 230000035945 sensitivity Effects 0.000 abstract description 6
- 238000002347 injection Methods 0.000 abstract 1
- 239000007924 injection Substances 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 108
- 101000639987 Homo sapiens Stearoyl-CoA desaturase 5 Proteins 0.000 description 6
- 102100033930 Stearoyl-CoA desaturase 5 Human genes 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 239000005864 Sulphur Substances 0.000 description 5
- 238000000354 decomposition reaction Methods 0.000 description 5
- 102100031948 Enhancer of polycomb homolog 1 Human genes 0.000 description 4
- 101000920634 Homo sapiens Enhancer of polycomb homolog 1 Proteins 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- 230000005477 standard model Effects 0.000 description 4
- 239000012159 carrier gas Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 description 2
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 2
- 206010070834 Sensitisation Diseases 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000003822 preparative gas chromatography Methods 0.000 description 2
- 230000008313 sensitization Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- XTQHKBHJIVJGKJ-UHFFFAOYSA-N sulfur monoxide Chemical compound S=O XTQHKBHJIVJGKJ-UHFFFAOYSA-N 0.000 description 2
- TXEYQDLBPFQVAA-UHFFFAOYSA-N tetrafluoromethane Chemical compound FC(F)(F)F TXEYQDLBPFQVAA-UHFFFAOYSA-N 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 239000012491 analyte Substances 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 238000011088 calibration curve Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000004590 computer program Methods 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000003745 diagnosis Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000004868 gas analysis Methods 0.000 description 1
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000012898 sample dilution Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 125000000475 sulfinyl group Chemical group [*:2]S([*:1])=O 0.000 description 1
- 150000003464 sulfur compounds Chemical class 0.000 description 1
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Abstract
The invention provides an SF6Gas chromatography detection systems and methods, the systems comprising: an electronic pressure flow controller EPC, a chromatographic column, a thermal conductivity detector TCD, a sulfur chemiluminescence detector SCD, a gas mixer, a sample injection valve, a switching valve and a quantitative ring. In carrying out the invention, gas chromatography is selected for SF6The qualitative and quantitative, accuracy and detection precision of the gas components are superior to those of the traditional detection means. Meanwhile, a sulfur chemiluminescence detector with the highest sulfur sensitivity is selected, and the detection precision can reach ppb level. Due to the equimolar response characteristic of the sulfur chemiluminescence detector SCD, the calibration of the sample is also simpler, more convenient and faster.
Description
Technical field
The present invention relates to power technology field, relate in particular to a kind of SF
6gas-chromatography detection system and method.
Background technology
Along with the high speed development of electric system, SF
6air insulating device is used widely because of advantages such as its operational reliability are high, floor area is little in actual motion.
Research shows, by analyzing SF
6gas composition can realize the detection and diagnosis of status of electric power.Conventional gas composition analytical approach comprises infra-red sepectrometry, gas sensor method, electrochemical process and dynamic ion analysis method etc.In infra-red sepectrometry, the characteristic peak of component is easily submerged in SF
6background peaks in, affect accuracy of detection.In gas sensor and electrochemical process, easily there is the interaction response between sour gas, affect the quantitative and qualitative analysis of component.
Summary of the invention
For solving the problems of the technologies described above, the invention provides a kind of SF
6gas-chromatography detection system, comprising: electron pressure flow controller EPC, chromatographic column, thermal conductivity detector (TCD) TCD, sulfur chemiluminescence detection device SCD, gas mixer, sampling valve, transfer valve, quantitative ring;
Described sampling valve is for gas sampling;
Described quantitative ring is arranged on described sampling valve, for accurately controlling gas sampling amount;
Described transfer valve is used for switching described SCD and described TCD;
Described EPC is connected with described sampling valve, for controlling described sampling valve to control by the gas flow of described chromatographic column;
Described chromatographic column is connected with described sampling valve, for separating of entering this SF through sampling valve
6the sample SF of gas-chromatography detection system
6gas and reference SF
6every component of gas;
Described TCD is connected with described transfer valve with described chromatographic column, for measuring respectively described reference SF
6gas and sample SF
6the content of non-sulfur component in gas, relatively reference SF
6gas and sample SF
6the conductivity of gas;
Described SCD is connected with described transfer valve, for measuring respectively described reference SF
6gas and sample SF
6the content of sulfur component in gas, and reference SF
6gas and sample SF
6chemiluminescent intensity when the carbon monoxide that gaseous combustion produces and ozone reaction;
Described gas mixer is connected with described sampling valve, for to sample SF
6gas dilutes.
Wherein, the temperature of described chromatographic column is controlled degree of adoption intensification.
Wherein, the flow control of described chromatographic column adopts constant current to control.
Wherein, described TCD and described SCD series connection.
Accordingly, the present invention also provides a kind of SF
6gas-chromatography detection method, described detection method is passed through SF as the aforementioned
6gas-chromatography detection system is realized, and comprising:
Described SF is set
6gas-chromatography detection system detects SF
6the parameter of component;
Adopt described SF
6gas-chromatography detection system analytic sample SF
6the component of gas, and adopt external standard method to set up described SF
6normal response curve;
Adopt SF
6gas-chromatography detection system is analyzed reference SF
6the appearance time of the component of gas and peak area, with described SF
6normal response curve is compared, to described reference SF
6the component of gas is carried out quantitative and qualitative analysis.
Wherein, described described SF is set
6gas-chromatography detection system detects SF
6the parameter of component, comprising:
The gas sampling mode that described sampling valve is set is split sampling, and its split ratio is 12:1;
The temperature that described chromatographic column is set is controlled degree of adoption intensification, and its flow control adopts constant current to control;
Described TCD and described SCD series connection are set, respectively to described reference SF
6gas detects.
Wherein, the described SF of described employing
6gas-chromatography detection system analytic sample SF
6the component of gas, and adopt external standard method to set up described SF
6normal response curve, comprising:
Measure respectively by described sampling valve and enter described SF
6the sample SF of the variable concentrations of gas-chromatography detection system
6the peak area of gas;
According to the peak area of described mensuration, draw described sample SF
6the normal response curve of the component of gas.
Wherein, described mensuration respectively by described sampling valve enters described SF
6the sample SF of the variable concentrations of gas-chromatography detection system
6the peak area of gas, comprising:
Described sample SF
6gas dilutes by described gas mixer;
Sample SF after dilution
6the quantitative ring that gas enters described sampling valve and is connected with described sampling valve, until described quantitative ring is full of sample SF
6gas;
Described EPC controls the sample SF in described quantitative ring
6gas is blown in described chromatographic column and analyzes, and measures its peak area.
Wherein, described employing SF
6gas-chromatography detection system is analyzed reference SF
6the appearance time of the component of gas and peak area, comprising:
Described reference SF
6the quantitative ring that gas enters described sampling valve and is connected with described sampling valve, until described quantitative ring is full of reference SF
6gas;
Described EPC controls the sample SF in described quantitative ring
6gas is blown in described chromatographic column and analyzes, and measures reference SF
6the appearance time of the component of gas and peak area.
Implement the present invention, select vapor-phase chromatography for SF
6the quantitative and qualitative analysis of gas composition, accuracy and accuracy of detection are all better than traditional detection means.Meanwhile, choose the highest sulfur chemiluminescence detection device of current sulphur sensitization sensitivity, accuracy of detection can reach ppb magnitude.Due to the equimolar response characteristic of sulfur chemiluminescence detection device SCD, the demarcation of sample is also more simple and efficient.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, to the accompanying drawing of required use in embodiment or description of the Prior Art be briefly described below, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skills, do not paying under the prerequisite of creative work, can also obtain according to these accompanying drawings other accompanying drawing.
Fig. 1 is a kind of SF provided by the invention
6the structural representation of gas-chromatography detection system.
Fig. 2 is a kind of SF provided by the invention
6the schematic flow sheet of gas-chromatography detection method embodiment mono-.
Fig. 3 is a kind of SF provided by the invention
6the schematic flow sheet of gas-chromatography detection method embodiment bis-.
Fig. 4 is a kind of SF provided by the invention
6the schematic flow sheet of gas-chromatography detection method embodiment tri-.
Fig. 5 is a kind of SF provided by the invention
6the schematic flow sheet of gas-chromatography detection method embodiment tetra-.
Fig. 6 is a kind of SF provided by the invention
6the schematic flow sheet of gas-chromatography detection method embodiment five.
Embodiment
The technical problem to be solved in the present invention is for the deficiency of detection means in the past, develops a kind ofly can accurately distinguish main gas decomposition components, comprises carbon tetrafluoride CF
4, sulfuretted hydrogen H
2s, fluorine sulfonyl SO
2f
2, fluoridize thionyl SOF
2, carbon disulphide CS
2, sulphuric dioxide SO
2, ten fluorine one oxidation two sulphur S
2oF
10deng detection method, and realize the accuracy of detection be low to moderate ppb magnitude simultaneously.
Referring to Fig. 1, be a kind of SF provided by the invention
6the structural representation of gas-chromatography detection system.
A kind of SF as shown in Figure 1
6gas-chromatography detection system, comprising:
Electron pressure flow controller EPC1, chromatographic column 2, thermal conductivity detector (TCD) TCD3, sulfur chemiluminescence detection device SCD4, gas mixer 5, sampling valve A, transfer valve B, quantitatively encircle 6;
Described sampling valve A is for gas sampling;
It is upper that described quantitative ring 6 is arranged on described sampling valve A, for accurately controlling gas sampling amount;
Described transfer valve B is used for switching described SCD4 and described TCD3;
Described EPC1 is connected with described sampling valve A, for controlling described sampling valve A to control by the gas flow of described chromatographic column 2;
Described chromatographic column 2 is connected with described sampling valve A, for separating of entering this SF through sampling valve A
6the sample SF of gas-chromatography detection system
6gas and reference SF
6every component of gas;
Described TCD3 is connected with described transfer valve B with described chromatographic column, for measuring respectively described reference SF
6gas and sample SF
6the content of non-sulfur component in gas, relatively reference SF
6gas and sample SF
6the conductivity of gas;
Described SCD4 is connected with described transfer valve B, for measuring respectively described reference SF
6gas and sample SF
6the content of sulfur component in gas, and reference SF
6gas and sample SF
6chemiluminescent intensity when the carbon monoxide that gaseous combustion produces and ozone reaction;
Described gas mixer 5 is connected with described sampling valve B, for to sample SF
6gas dilutes.
In specific implementation, EPC1 is accurate to be controlled by the SF of chromatographic column 2
6gas flow, can keep stable, post flow constant of minute flowing pressure.Chromatographic column 2 is for being applicable to the GS-GASPRO capillary column of analysis of sulfur compounds, and its length is 60m, and column diameter 0.320mm, for SF
6in the separation of every component.TCD3 is for SF
6in not sulfur component as the mensuration of CF4 and air, reference SF relatively
6gas and sample SF
6the conductivity of gas, its sensitivity can reach 2500mVml/mg, and the range of linearity is greater than 104, possesses linear response characteristic.SCD4 is for reference SF
6gas and sample SF
6the mensuration of sulfur component in gas, chemiluminescent intensity when the sulfur monoxide that the burning of measurement analyte produces and ozone reaction, sensitivity can reach 0.5pgS/sec, and the range of linearity is greater than 104, possesses linear response, sulphur selection response characteristic and equimolar response characteristic simultaneously.Gas mixer 5 is for the dilution of standard model.Sampling valve A, transfer valve B are six-way valve, are respectively used to the switching of gas sampling and detecting device.Quantitatively the specification of ring 6 is that 0.25mL/1mL/2mL is optional, for accurately controlling the sample size that enters sampling valve A.This SF
6sampling valve A, transfer valve B in gas-chromatography detection system, quantitatively encircle 6 and pipeline all through sulfur passivation, process, to reduce the impact of gas circuit on testing result.
Accordingly, the present invention also provides a kind of SF
6gas-chromatography detection method, described detection method is by aforesaid SF
6gas-chromatography detection system is realized.
SF shown in Figure 2
6the schematic flow sheet of gas-chromatography detection method embodiment mono-, it comprises:
SF shown in Figure 3
6the schematic flow sheet of gas-chromatography detection method embodiment bis-, in the present embodiment two, arranges described SF by specific descriptions
6gas-chromatography detection system detects SF
6the flow process of the parameter of component, comprising:
It should be noted that, split sampling is a kind of conventional operator scheme of shunting/Splitless injecting samples mouth, refers to sample and is divided into two parts, and sub-fraction sample enters chromatographic column, and most of sample exports discharge by shunting.For example, split ratio 12:1 is in 13 duplicate samples has 1 part to enter chromatographic column.Split ratio is larger, and the response of same sample in chromatogram is just less.Split ratio is too small can cause that sample peak shape is poor, affects the Measurement accuracy of peak area, also likely causes the saturated of SCD detecting device simultaneously.
Concrete, the temperature of chromatographic column is controlled and is selected degree temperature-raising method, and its single heating schedule 20min consuming time is set, and is divided into following three phases: 1. initial temperature is 35 ℃, keeps 2min; 2. 5 ℃/min of heating rate, 100 ℃ of finishing temperatures, heating-up time 13min; 3. 100 ℃ keep 5min.Constant current control mode is selected in chromatographic column flow control, and column flow rate is set as 5mL/min.
In specific implementation, TCD, SCD are set to the mode of Series detectors.TCD well heater is set as to 200 ℃, reference flow 15mL/min, tail wind drift amount 5mL/min.SCD well heater is set as to 200 ℃, and chamber temperature is 800 ℃, and chamber pressure is 3-10 torr (Torr), and the ozone flow by rear ozone damper is at 3-6psi.Mixed sample testing result shows, under the method, the degree of separation of SF6 and decomposition components thereof is more excellent.
SF shown in Figure 4
6the schematic flow sheet of gas-chromatography detection method embodiment tri-, in the present embodiment three, will describe the described SF of described employing
6gas-chromatography detection system analytic sample SF
6the component of gas, and adopt external standard method to set up described SF
6the flow process of normal response curve, comprising:
It should be noted that, external standard method is also referred to as calibration curve method.In specific implementation, get the standard model SF of a series of variable concentrations
6gas, accurately controls identical sample size, measures respectively peak area (or peak height), with corresponding peak area, concentration of component is mapped, and can obtain the typical curve of this component.While doing typical curve, should note the range of linearity of response, the TCD selecting in this method and the SCD range of linearity are wider, and measurement range internal standard curve is linearity.
When component concentration variation range is little, can adopt Single Point Correction Method, be specially a standard sample close with tested concentration of component of preparation, the concentration of standard sample is Cs, get respectively standard sample and the sample analysis of same amount, from the chromatogram obtaining, measure both peak area As and Ai(or peak height), by formula (1), calculate the volume fraction of tested component.
C
ifor the volume fraction of this component in sample, Cs is the volume fraction of component in standard sample.
That the external standard method that the embodiment of the present invention provides has is easy, advantage fast.Accuracy is higher, is applicable to the express-analysis of sample in enormous quantities.
SF shown in Figure 5
6the schematic flow sheet of gas-chromatography detection method embodiment tetra-, in the present embodiment four, enters described SF by described the mensuration respectively by described sampling valve of detailed description
6the sample SF of the variable concentrations of gas-chromatography detection system
6the peak area of gas, comprising:
In specific implementation, gas mixer provided by the invention can be realized the dilution of high concentration standard model designated ratio.Sample SF in dress sample process
6total gas flow rate can be recorded by the precise electronic flowmeter that is arranged on the 1 mouthful of place of the sampling valve A shown in Fig. 1.Dilute sample SF
6the detailed process of gas is: open standard specimen source needle-valve, close dilution carrier gas, record sample SF when undiluted
6total gas flow rate, then keeps standard specimen source needle-valve constant, utilizes EPC to regulate the flow of carrier gas for dilution, sample SF during record dilution
6total gas flow rate.Diluting forward and backward throughput ratio is sample SF
6the dilution ratio of gas, can calculate in quantitative ring sample SF after dilution in conjunction with the concentration of standard specimen
6the concentration of gas.This lays the foundation for the mensuration of variable concentrations standard model.
That during Criterion response curve, take is drive in the wrong direction gas circuit connected mode, i.e. sample SF
6gas during by sampling valve A through gas mixer 5 by 2 mouthfuls enter, 1 mouthful emptying.When sampling valve A closes (as accompanying drawing 1 shows), sample SF
6gas via 2 mouthfuls-3 mouthfuls of sampling valve A-quantitatively encircle-6 mouthfuls-1 mouthful of 6-sampling valve A, finally by emptying by 1 mouthful.As sample SF
6gas is full of quantitative ring 6, and after immediate shipment sample, sampling valve A is rotated counterclockwise 60 ° and opens, and the part of six-way valve conducting originally disconnects now, the present conducting of part originally disconnecting.By EPC1, precisely controlled the carrier gas of flow, via 5 mouthfuls-6 mouthfuls of sampling valve A-quantitative 3 mouthfuls-4 mouthfuls of ring-sampling valve A, by quantitatively encircling standard specimen in 6, be blown in chromatographic column 2 and analyze.When sample SF6 gas all enters after chromatographic column, sampling valve A turns clockwise 60 ° and closes, and restarts the dress sample of next round.In this method, sampling valve A opens when capture program operation 0.01min, during 1min, closes.
SF shown in Figure 6
6the schematic flow sheet of gas-chromatography detection method embodiment tetra-, in the present embodiment five, will describe described employing SF in detail
6gas-chromatography detection system is analyzed reference SF
6the appearance time of the component of gas and the flow process of peak area, comprising:
It should be noted that, gas mixer 5 is only done Sample Dilution use when Criterion response curve, while analyzing testing sample, need disconnect with detection system.
The reference SF of above-mentioned steps 500 and step 501
6direct motion gas circuit connected mode is taked in gas analysis, and through sampling valve A when reference SF6 gas is by sampling valve A 1 mouthful enters, emptying by 2 mouthfuls.Dress sample and sample presentation are to process and the sample SF of chromatographic column 2
6identical during eudiometry.For keeping the sulphur detection sensitivity of SCD4, in mensuration process, should avoid high-concentration sulfur-containing compound (SF
6substrate gas) a large amount of inflows.At SF
6go out before peak, transfer valve B closes (as accompanying drawing 1 shows), reference SF
6the path of gas is TCD3-4 mouth-5 mouthful-SCD4.Work as SF
6go out peak and decomposition components while not yet going out peak, transfer valve B is rotated counterclockwise 60 ° and opens, reference SF
6gas is mouthful emptying via TCD3-4 mouth-3.When decomposition components goes out peak, transfer valve B turns clockwise 60 ° and closes, reference SF
6gas is back in SCD4 and analyzes.In this method, transfer valve B opens when capture program operation 2.5min, during 6.8min, closes.
Record reference SF
6the appearance time of each component and peak area in gas, relatively realize SF with the normal response curve of aforementioned foundation
6the quantitative and qualitative analysis of middle gas composition.
SF
6gas decomposition components common in power equipment (comprises CF
4, H
2s, SO
2f
2, SOF
2, CS
2, SO
2, S
2oF
10deng) all can be detected by system and method provided by the invention, the accurate quantitative analysis limit of each component is as shown in table 1.
Table 1 gas composition and accurate quantitative analysis limit thereof
Implement the present invention, select vapor-phase chromatography for SF
6the quantitative and qualitative analysis of gas composition, accuracy and accuracy of detection are all better than traditional detection means.Meanwhile, choose the highest sulfur chemiluminescence detection device of current sulphur sensitization sensitivity, accuracy of detection can reach ppb(parts per billion, part per billion) magnitude.Due to the equimolar response characteristic of sulfur chemiluminescence detection device SCD, the demarcation of sample is also more simple and efficient.
One of ordinary skill in the art will appreciate that all or part of flow process realizing in above-described embodiment method, to come the hardware that instruction is relevant to complete by computer program, described program can be stored in a computer read/write memory medium, this program, when carrying out, can comprise as the flow process of the embodiment of above-mentioned each side method.Wherein, described storage medium can be magnetic disc, CD, read-only store-memory body (Read-Only Memory, ROM) or random store-memory body (Random Access Memory, RAM) etc.
Above content is in conjunction with concrete preferred implementation further description made for the present invention, can not assert that specific embodiment of the invention is confined to these explanations.For general technical staff of the technical field of the invention, without departing from the inventive concept of the premise, can also make some simple deduction or replace, all should be considered as belonging to protection scope of the present invention.
Claims (9)
1. a SF
6gas-chromatography detection system, is characterized in that, comprising: electron pressure flow controller EPC, chromatographic column, thermal conductivity detector (TCD) TCD, sulfur chemiluminescence detection device SCD, gas mixer, sampling valve, transfer valve, quantitative ring;
Described sampling valve is for gas sampling;
Described quantitative ring is arranged on described sampling valve, for accurately controlling gas sampling amount;
Described transfer valve is used for switching described SCD and described TCD;
Described EPC is connected with described sampling valve, for controlling described sampling valve to control by the gas flow of described chromatographic column;
Described chromatographic column is connected with described sampling valve, for separating of entering this SF through sampling valve
6the sample SF of gas-chromatography detection system
6gas and reference SF
6every component of gas;
Described TCD is connected with described transfer valve with described chromatographic column, for measuring respectively described reference SF
6gas and sample SF
6the content of non-sulfur component in gas, relatively reference SF
6gas and sample SF
6the conductivity of gas;
Described SCD is connected with described transfer valve, for measuring respectively described reference SF
6gas and sample SF
6the content of sulfur component in gas, and reference SF
6gas and sample SF
6chemiluminescent intensity when the carbon monoxide that gaseous combustion produces and ozone reaction;
Described gas mixer is connected with described sampling valve, for to sample SF
6gas dilutes.
2. SF as claimed in claim 1
6gas-chromatography detection system, is characterized in that, the temperature of described chromatographic column is controlled degree of adoption and heated up.
3. SF as claimed in claim 2
6gas-chromatography detection system, is characterized in that, the flow control of described chromatographic column adopts constant current to control.
4. SF as claimed in claim 3
6gas-chromatography detection system, is characterized in that, described TCD and described SCD series connection.
5. a SF
6gas-chromatography detection method, is characterized in that, described detection method is by the SF as described in any one in claim 1 to 4
6gas-chromatography detection system is realized, and comprising:
Described SF is set
6gas-chromatography detection system detects SF
6the parameter of component;
Adopt described SF
6gas-chromatography detection system analytic sample SF
6the component of gas, and adopt external standard method to set up described SF
6normal response curve;
Adopt SF
6gas-chromatography detection system is analyzed reference SF
6the appearance time of the component of gas and peak area, with described SF
6normal response curve is compared, to described reference SF
6the component of gas is carried out quantitative and qualitative analysis.
6. SF as claimed in claim 5
6gas-chromatography detection method, is characterized in that, described described SF is set
6gas-chromatography detection system detects SF
6the parameter of component, comprising:
The gas sampling mode that described sampling valve is set is split sampling, and its split ratio is 12:1;
The temperature that described chromatographic column is set is controlled degree of adoption intensification, and its flow control adopts constant current to control;
Described TCD and described SCD series connection are set, respectively to described reference SF
6gas detects.
7. SF as claimed in claim 6
6gas-chromatography detection method, is characterized in that, the described SF of described employing
6gas-chromatography detection system analytic sample SF
6the component of gas, and adopt external standard method to set up described SF
6normal response curve, comprising:
Measure respectively by described sampling valve and enter described SF
6the sample SF of the variable concentrations of gas-chromatography detection system
6the peak area of gas;
According to the peak area of described mensuration, draw described sample SF
6the normal response curve of the component of gas.
8. SF as claimed in claim 7
6gas-chromatography detection method, is characterized in that, described mensuration respectively by described sampling valve enters described SF
6the sample SF of the variable concentrations of gas-chromatography detection system
6the peak area of gas, comprising:
Described sample SF
6gas dilutes by described gas mixer;
Sample SF after dilution
6the quantitative ring that gas enters described sampling valve and is connected with described sampling valve, until described quantitative ring is full of sample SF
6gas;
Described EPC controls the sample SF in described quantitative ring
6gas is blown in described chromatographic column and analyzes, and measures its peak area.
9. SF as claimed in claim 7
6gas-chromatography detection method, is characterized in that, described employing SF
6gas-chromatography detection system is analyzed reference SF
6the appearance time of the component of gas and peak area, comprising:
Described reference SF
6the quantitative ring that gas enters described sampling valve and is connected with described sampling valve, until described quantitative ring is full of reference SF
6gas;
Described EPC controls the sample SF in described quantitative ring
6gas is blown in described chromatographic column and analyzes, and measures reference SF
6the appearance time of the component of gas and peak area.
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| CN104198638A (en) * | 2014-08-20 | 2014-12-10 | 国家电网公司 | Chromatographic analysis system and method for detecting sulfur hexafluoride decomposition products |
| CN104198638B (en) * | 2014-08-20 | 2015-11-18 | 国家电网公司 | A kind of chromatographic analysis system and method detecting sulfur hexafluoride decomposition product |
| CN106153431A (en) * | 2016-07-21 | 2016-11-23 | 中国科学院山西煤炭化学研究所 | The detection method of a kind of quick mensuration raw gas composition and device thereof |
| CN106290652A (en) * | 2016-09-21 | 2017-01-04 | 国家电网公司 | A kind of detection equipment for oil-filled equipment is detected |
| CN106290652B (en) * | 2016-09-21 | 2019-05-24 | 国家电网公司 | A kind of detection device for being detected to oil-filled equipment |
| CN110214269A (en) * | 2017-03-15 | 2019-09-06 | 株式会社岛津制作所 | Chemiluminescence detector reaction unit and the chemiluminescence detector and chemical luminescence detection method for having the reaction unit |
| CN109085280A (en) * | 2018-10-16 | 2018-12-25 | 广东电网有限责任公司 | A kind of system of quantitative detection sulfur hexafluoride gas ingredient |
| CN109085280B (en) * | 2018-10-16 | 2024-04-12 | 广东电网有限责任公司 | System for quantitatively detecting sulfur hexafluoride gas component |
| CN110808203A (en) * | 2019-11-12 | 2020-02-18 | 北京中计新科仪器有限公司 | Device and method for quickly and accurately detecting impurities in high-purity hydrogen for hydrogen fuel cell |
| CN110808203B (en) * | 2019-11-12 | 2022-03-18 | 北京中计新科仪器有限公司 | Device and method for quickly and accurately detecting impurities in high-purity hydrogen for hydrogen fuel cell |
| CN111398484A (en) * | 2020-04-27 | 2020-07-10 | 深圳供电局有限公司 | Used for detecting SF in transformer oil dissolved gas6Gas chromatograph |
| CN111398484B (en) * | 2020-04-27 | 2022-04-08 | 深圳供电局有限公司 | Used for detecting SF in transformer oil dissolved gas6Gas chromatograph |
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