CN108088892A - A kind of SF6On-line rapid measurement device and method - Google Patents
A kind of SF6On-line rapid measurement device and method Download PDFInfo
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- CN108088892A CN108088892A CN201611044508.7A CN201611044508A CN108088892A CN 108088892 A CN108088892 A CN 108088892A CN 201611044508 A CN201611044508 A CN 201611044508A CN 108088892 A CN108088892 A CN 108088892A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
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Abstract
The invention discloses a kind of SF in atmospheric environment6Carry out new method that is sensitive, quickly monitoring on-line and device.This method utilizes negative ion mode ion mobility spectrometry, detects the SF in dry environment and different humidity environment by way of direct injected and doping steam respectively6.Monitoring device includes：Float gas, mass flowmenter, air filter, dopant bottle, dopant, spectrometric system, amplifier, vacuum pump etc..The present invention is sampled by negative ion mode ion mobility spectrometry air-breathing, and the mode of the steam of design dopant device doping certain concentration triggers chemical reaction, while different humidity in excluding atmospheric environment disturbs measurement, by monitoring SF6Molecular ion peak and the new peak that is formed after being reacted with steam, improve ion mobility spectrometry to SF6The Stability and veracity of measurement.Present invention detection limit is up to 0.1ppm.
Description
Technical field
The invention belongs to Ion mobility spectrometry fields.It is sampled by negative ion mode ion mobility spectrometry air-breathing, design is mixed
The mode of the steam of miscellaneous dose of device doping certain concentration, triggers chemical reaction, different humidity is to measurement in atmospheric environment is excluded
While interference, by monitoring SF6Molecular ion peak and the new peak that is formed after being reacted with steam, improve ion mobility spectrometry to SF6
The Stability and veracity of measurement.
Background technology
Global about 8500 tons of SF of production every year6Gas, wherein 80% is used for mesohigh power equipment.With SF6A large amount of make
With SF6The continuous proposition for the problems such as leakage is to the threat of service personnel's life and health, electric power safety operation hidden danger, greenhouse effects,
National relevant regulations, such as《Sulfur hexafluoride electrical equipment operation, experiment and service personnel's security protection detailed rules and regulations》(DL/T639-
1997)、《The guide for processing and measuring SF6 gas in power apparatus》(GB 8905-1996)、《Electrical safe working order》
(DL408-91) etc., it is desirable that apply SF in electric system gas-insulated switchgear etc.6Workplace, SF will be installed6Gas
Leakage monitoring equipment.
SF6The links such as use, preservation in, it is desirable that the content of stringent limitation moisture.Because moisture can not only influence electric power
The insulation performance of equipment, moreover it is possible under the action of electric arc, with SF6Generate fluoride, such as HF, SOF4Deng.But aqueous vapor is air
One important composition of environment, with the variation of space-time, relative humidity difference is also very big.The SF being leaked in environment6Unavoidably
To influence instrument to SF with gas-vapor mix in air environment and reaction6Measurement.
The present invention is based on Ion mobility spectrometry, the mode of the steam of design dopant device doping certain concentration triggers
Chemical reaction, by monitoring SF6Molecular ion peak and the peak that is formed after being reacted with steam, it is different in atmospheric environment so as to exclude
Humidity disturbs measurement.
The content of the invention
It is an object of the invention to provide a kind of SF6On-line rapid measurement method and device.
A kind of SF6On-line rapid measurement method and device include：Float gas, mass flowmenter, sample gas, air filtration
Device, triple valve, dopant bottle, dopant, spectrometric system, amplifier, mass flowmenter, vacuum pump, tail gas.
Technical solution is：Sample gas is connected with air inlet of the air filter directly with dopant bottle top, dopant bottle
The gas outlet on top is connected with the injection port of spectrometric system；The tail gas mouth of spectrometric system through mass flowmenter with
The air inlet of vacuum pump is connected.Drift gas be clean air, through mass flowmenter with certain flow by float gas port enter from
In son migration spectra system；By the effect of vacuum pump, sample gas enters ion through air filter directly or by dopant bottle
It migrates in spectra system；Tail gas is discharged through mass flowmenter by vacuum pump.
Atmospheric sample, by air filter, removes the particulate matter in atmospheric environment before migration tube is entered.
Conduit is four fluorine tube used by gas circuit, to reduce SF6Residual.
Mass flowmenter measures the flow of drift gas and tail gas respectively, and the difference of the two flow is sample gas sampling quantity.
Flow adjustment range is respectively 10mL/min~500mL/min and 10mL/min~1000mL/min.By adjusting
Difference between two mass flowmenters to control sample size, achievees the purpose that expand spectrometric system measurement range.Dynamically
Measurement range is more than 3 orders of magnitude, and minimum detection limit is up to 0.1ppm.
There is constant temperature system outside dopant bottle, the inside of dopant bottle is made to maintain at a certain temperature.Dopant is pure
Water.Under the action of constant temperature system, in the entrance sample gas that the dopant in dopant bottle passes through air hole.Wherein dopant is
Pure water.
By monitoring SF6Molecular ion peak and the peak that is formed after being reacted with steam, avoid different humidity in atmospheric environment
Interference to measurement.
SF is made by the ion mobility spectrometry peak position and peak intensity for the sample for measuring doping steam6It is able to accurate qualitative.Pass through
The Ion transfer spectral strength of the sample of measurement doping steam makes SF6It is able to accurate quantification.
Advantages of the present invention is as follows：
The present invention is based on Ion mobility spectrometry, high sensitivity, measuring speed are fast, cost-effective, easy to operate.Using pure
Water purification is dopant, and instrument operating cost is low, pollution-free, is suitble to long-term on-line monitoring.
Description of the drawings
Fig. 1 is On-line rapid measurement SF6Installation drawing.Wherein, 1 is the first mass flowmenter for drift gas, 2, and 3 be sample
Gas, 4 be air filter, and 5 be dopant bottle, and 6 be dopant, and 7 be spectrometric system, and 8 be amplifier, and 9 adopt for signal
Collection and display device, 10 be the second mass flowmenter, and 11 be vacuum pump, and 12 be tail gas；
Fig. 2 is the SF under measurement dry environment6Ion transfer spectrogram
Fig. 3 is the SF under measurement different humidity environment6Ion transfer spectrogram
Specific embodiment
Following embodiment illustrates the use of the present invention, but does not limit the application range.
Embodiment 1
Work as SF6When On-line rapid measurement device works, migration area voltage is set to 400V/cm, and drift throughput is set to 400ml/
Min, exhaust flow are set to 600ml/min, and sampling quantity is 200ml/min.When cleaned air of the sample for drying, ion moves
There are one reagent reacting quasi-molecular ions only at 5.58ms in shifting spectrogram.When containing SF in dry cleaned air6During gas, not only
There are one reagent reacting quasi-molecular ions at 5.58ms, also occurs SF at 6.44ms6Molecular ion peak.It is empty to measure dry environment
Contain SF in gas6The ion transfer spectrogram of gas is shown in Fig. 2.
Embodiment 2
Aqueous vapor is an important composition of atmospheric environment.When there is steam in environment, except reagent in ion transfer spectrogram
Quasi-molecular ions, SF6Outside molecular ion peak, occurs a new peak at 6.18ms, intensity enhances with the increase of humidity.Actually should
With the variation of space-time in, relative humidity difference is also very big, general RH ＞ 30%, therefore, doping steam make sample gas all in
Under high humidity environment, by the peak at 6.18ms to SF6It is detected.Device is measured under the same conditions under different humidity environment
The SF of (RH=0%, 20%, 40%, 60%, 80%)6Gas is shown in Fig. 3.
Embodiment 3
When making dopant without water, since the range of humidity variation in atmospheric environment is larger, ion mobility spectrometry is to SF6
The response intensity at peak differs at 6.18ms, it is difficult to realize to SF6Measurement, as shown in Figure 3.
Embodiment 4
During 35 DEG C of the temperature range of dopant bottle constant temperature, the humidity of sample gas can maintain more than 70%, at this time in difference
The SF of same concentrations under humidity6The response intensity at peak is basically identical at 6.18ms.
Claims (10)
1. a kind of SF6On-line rapid measurement device, it is characterised in that：
Device includes：Drift gas (1), the first mass flowmenter (2), air filter (4), dopant bottle (5), are mixed at sample gas (3)
Miscellaneous dose (6), spectrometric system (7), signal amplifier (8), signal acquisition and display device (9), the second mass flowmenter
(10), vacuum pump (11), tail gas (12)；
Spectrometric system (7) gas circuit includes drift gas port, injection port, tail gas mouth；The drift gas (1) in gas source of the gas is floated through the first matter
Amount flowmeter (2) is connected with spectrometric system (7) drift gas port；Sample gas (3) and air filter (4) are directly and dopant
The air inlet on bottle (5) top is connected, and the gas outlet on dopant bottle (5) top is connected with the injection port of spectrometric system (7)；
It is offered on the closed container that internal filling dopant (6) is placed in dopant bottle (5), closed container top as ventilative
The through hole in hole；
Air inlet of the tail gas (12) of spectrometric system (7) tail gas mouth through the second mass flow (10) meter with vacuum pump (11)
It is connected；Tail gas (12) is discharged through mass flowmenter (10) by vacuum pump (11)；
The electric signal of spectrometric system (7) output is gathered after signal amplifier (8) by signal acquisition and display device (9)
And it exports.
2. the apparatus according to claim 1, it is characterised in that：Electric heater unit is equipped with outside dopant bottle (5)；The electricity
Heating unit refers to：Dopant bottle (5) is placed in an electric heating cover or in water bath or in oil bath or in dopant bottle (5)
Wall surface be equipped with electric heating wire, electric heating tube or heat tape；
Temperature thermocouple is equipped in the side wall surface of dopant bottle (5), temperature thermocouple passes through conducting wire and temperature controller signal
Connection, electric heater unit are connected through temperature controller with external circuit.
3. the apparatus according to claim 1, it is characterised in that：Air filter (4) is to be filtered using polytetrafluoroethylene (PTFE) micropore
Film is the air filter of filter membrane.
4. a kind of SF using any described devices of claim 1-36On-line rapid measurement method, it is characterised in that：
It is clean air to float gas (1), is entered through mass flowmenter (2) by floating gas port in spectrometric system (7)；
SF containing known concentration6Air and/or nitrogen be standard specimen gas, standard specimen gas is through air filter (4) except leading to after solid particulate matter
Into SF in progress standard specimen gas in spectrometric system after overdoping agent bottle (5) constant temperature and humidity6The measurement of content obtains standard specimen
The ion transfer spectrogram of gas；
Sample gas through air filter (4) except after solid particulate matter by dopant bottle (5) constant temperature and humidity after enter Ion transfer
SF in sample is carried out in spectra system6The measurement of content obtains the ion transfer spectrogram of sample gas；It is used and mark when sample gas measures
The condition of same constant temperature and humidity when sample gas measures；
The ion transfer spectrogram of sample gas and the ion transfer spectrogram of standard specimen gas are compared, obtain SF in sample gas6Concentration.
5. SF according to claim 46On-line rapid measurement method, it is characterised in that：Sample is into ion mobility spectrometry
By air filter (4) before system (7), the particulate matter in sample is removed, avoids making the inside of spectrometric system (7)
Into pollution.
6. SF according to claim 46On-line rapid measurement method, it is characterised in that：
Tri- tunnels of spectrometric system (7) work gas circuit Gong Wei, that is, float gas, sample gas, tail gas；Work in vacuum pump (11)
Under, drift gas (1) and sample gas (3) are inhaled into spectrometric system (7), while are divided with mass flowmenter (2) and (10)
The flow of gas and tail gas Ce Liang not be floated, the difference of the two flow is sample gas (3) sampling quantity；Tail gas (12) after measured by
Vacuum pump (11) is discharged.
7. SF according to claim 46On-line rapid measurement method, it is characterised in that：Dopant bottle (6) is external persevering
Warm system makes the inside of dopant bottle (6) maintain at a certain temperature, to be fixed with the band for containing dopant in dopant bottle (6)
The closed container (6) of air hole；Wherein dopant is pure water.
8. SF according to claim 16On-line rapid measurement method, it is characterised in that：By measuring constant-humidity constant-temperature sample
Ion mobility spectrometry peak position make SF6It is able to accurate qualitative；By the Ion transfer spectral strength for measuring doping constant-humidity constant-temperature sample
Make SF6It is able to accurate quantification；By monitoring SF6Molecular ion peak and the new peak that is formed after being reacted with steam, exclude atmospheric environment
The interference of middle different humidity (RH=0%-100%).
9. SF according to claim 66On-line rapid measurement method, it is characterised in that：By adjusting mass flowmenter
(2) difference between mass flowmenter (10) to control sample size, reaches and expands spectrometric system (7) measurement range
Purpose.
10. SF according to claim 46On-line rapid measurement method, it is characterised in that：The temperature of dopant bottle (5) constant temperature
Spend 35-60 DEG C of scope, preferably 40-50 DEG C；The RH range 50-95% of constant humidity, preferably 70-90%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611044508.7A CN108088892A (en) | 2016-11-21 | 2016-11-21 | A kind of SF6On-line rapid measurement device and method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611044508.7A CN108088892A (en) | 2016-11-21 | 2016-11-21 | A kind of SF6On-line rapid measurement device and method |
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| CN108088892A true CN108088892A (en) | 2018-05-29 |
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| CN201611044508.7A Pending CN108088892A (en) | 2016-11-21 | 2016-11-21 | A kind of SF6On-line rapid measurement device and method |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110988208A (en) * | 2019-12-18 | 2020-04-10 | 中科新天地（合肥）环保科技有限公司 | VOCs check out test set based on ion mobility spectrometry |
| CN111024798A (en) * | 2019-12-12 | 2020-04-17 | 天津科技大学 | System and method for automatically monitoring environment dimethyl sulfur on line |
| CN111239234A (en) * | 2018-11-29 | 2020-06-05 | 中国科学院大连化学物理研究所 | Non-radioactive method for on-line monitoring of ammonia gas |
| CN112986373A (en) * | 2019-12-12 | 2021-06-18 | 中国科学院大连化学物理研究所 | Ion mobility spectrometry and application thereof |
| CN114627625A (en) * | 2020-12-10 | 2022-06-14 | 中国科学院大连化学物理研究所 | Early warning device and method for dangerous chemical leakage |
| CN115183152A (en) * | 2022-07-26 | 2022-10-14 | 中国科学院大连化学物理研究所 | Control gas circuit of pumping gas injection ion mobility spectrometer |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111239234A (en) * | 2018-11-29 | 2020-06-05 | 中国科学院大连化学物理研究所 | Non-radioactive method for on-line monitoring of ammonia gas |
| CN111024798A (en) * | 2019-12-12 | 2020-04-17 | 天津科技大学 | System and method for automatically monitoring environment dimethyl sulfur on line |
| CN112986373A (en) * | 2019-12-12 | 2021-06-18 | 中国科学院大连化学物理研究所 | Ion mobility spectrometry and application thereof |
| CN111024798B (en) * | 2019-12-12 | 2023-04-28 | 天津科技大学 | System and method for automatically monitoring environment dimethyl sulfide on line |
| CN110988208A (en) * | 2019-12-18 | 2020-04-10 | 中科新天地（合肥）环保科技有限公司 | VOCs check out test set based on ion mobility spectrometry |
| CN110988208B (en) * | 2019-12-18 | 2022-03-11 | 中科新天地（合肥）环保科技有限公司 | VOCs check out test set based on ion mobility spectrometry |
| CN114627625A (en) * | 2020-12-10 | 2022-06-14 | 中国科学院大连化学物理研究所 | Early warning device and method for dangerous chemical leakage |
| CN115183152A (en) * | 2022-07-26 | 2022-10-14 | 中国科学院大连化学物理研究所 | Control gas circuit of pumping gas injection ion mobility spectrometer |
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Application publication date: 20180529 |