CN114813448A - Method for automatically testing fluorine content in fluorine-nitrogen mixed gas - Google Patents
Method for automatically testing fluorine content in fluorine-nitrogen mixed gas Download PDFInfo
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- 239000011737 fluorine Substances 0.000 title claims abstract description 95
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- 238000000034 method Methods 0.000 title claims abstract description 47
- YPDSOAPSWYHANB-UHFFFAOYSA-N [N].[F] Chemical compound [N].[F] YPDSOAPSWYHANB-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 238000012360 testing method Methods 0.000 title claims abstract description 42
- 238000001179 sorption measurement Methods 0.000 claims abstract description 64
- 238000006243 chemical reaction Methods 0.000 claims abstract description 25
- 238000010521 absorption reaction Methods 0.000 claims abstract description 4
- 230000001105 regulatory effect Effects 0.000 claims description 20
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 17
- 238000010926 purge Methods 0.000 claims description 17
- 230000008569 process Effects 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 7
- 239000000945 filler Substances 0.000 claims description 6
- 238000010408 sweeping Methods 0.000 claims 2
- 230000008859 change Effects 0.000 abstract description 6
- 238000004458 analytical method Methods 0.000 description 13
- 230000009286 beneficial effect Effects 0.000 description 12
- 238000005259 measurement Methods 0.000 description 7
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 5
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 5
- 239000000292 calcium oxide Substances 0.000 description 5
- 239000004033 plastic Substances 0.000 description 5
- 229920003023 plastic Polymers 0.000 description 5
- 238000011084 recovery Methods 0.000 description 5
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 4
- 229910001634 calcium fluoride Inorganic materials 0.000 description 4
- 239000000460 chlorine Substances 0.000 description 4
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- 230000006378 damage Effects 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 238000012856 packing Methods 0.000 description 4
- 238000004364 calculation method Methods 0.000 description 3
- 239000003638 chemical reducing agent Substances 0.000 description 3
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- 229910044991 metal oxide Inorganic materials 0.000 description 3
- 150000004706 metal oxides Chemical class 0.000 description 3
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- WTEOIRVLGSZEPR-UHFFFAOYSA-N boron trifluoride Chemical compound FB(F)F WTEOIRVLGSZEPR-UHFFFAOYSA-N 0.000 description 2
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- 238000003682 fluorination reaction Methods 0.000 description 2
- 238000004868 gas analysis Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- KWVVTSALYXIJSS-UHFFFAOYSA-L silver(ii) fluoride Chemical compound [F-].[F-].[Ag+2] KWVVTSALYXIJSS-UHFFFAOYSA-L 0.000 description 2
- 231100000167 toxic agent Toxicity 0.000 description 2
- 239000003440 toxic substance Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910015900 BF3 Inorganic materials 0.000 description 1
- 229910021583 Cobalt(III) fluoride Inorganic materials 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 1
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- WZJQNLGQTOCWDS-UHFFFAOYSA-K cobalt(iii) fluoride Chemical compound F[Co](F)F WZJQNLGQTOCWDS-UHFFFAOYSA-K 0.000 description 1
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- 238000003379 elimination reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002222 fluorine compounds Chemical class 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 1
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- 238000007689 inspection Methods 0.000 description 1
- 229910052743 krypton Inorganic materials 0.000 description 1
- DNNSSWSSYDEUBZ-UHFFFAOYSA-N krypton atom Chemical compound [Kr] DNNSSWSSYDEUBZ-UHFFFAOYSA-N 0.000 description 1
- GJOMWUHGUQLOAC-UHFFFAOYSA-L magnesium difluoride hydrofluoride Chemical compound [H+].[F-].[F-].[F-].[Mg++] GJOMWUHGUQLOAC-UHFFFAOYSA-L 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052754 neon Inorganic materials 0.000 description 1
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- SFZCNBIFKDRMGX-UHFFFAOYSA-N sulfur hexafluoride Chemical compound FS(F)(F)(F)(F)F SFZCNBIFKDRMGX-UHFFFAOYSA-N 0.000 description 1
- 229960000909 sulfur hexafluoride Drugs 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- SANRKQGLYCLAFE-UHFFFAOYSA-H uranium hexafluoride Chemical compound F[U](F)(F)(F)(F)F SANRKQGLYCLAFE-UHFFFAOYSA-H 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N7/00—Analysing materials by measuring the pressure or volume of a gas or vapour
- G01N7/02—Analysing materials by measuring the pressure or volume of a gas or vapour by absorption, adsorption, or combustion of components and measurement of the change in pressure or volume of the remainder
- G01N7/04—Analysing materials by measuring the pressure or volume of a gas or vapour by absorption, adsorption, or combustion of components and measurement of the change in pressure or volume of the remainder by absorption or adsorption alone
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Abstract
The patent discloses a method for automatically testing the fluorine content in a fluorine-nitrogen mixed gas; the device comprises an air supply device, a metering device, an adsorption device and a vacuum device. The metering device, the adsorption device and the vacuum device are connected in sequence through a pipeline, a hand valve and a flow-limiting orifice plate. The measured fluorine-nitrogen mixed gas is introduced into the absorption device to react, the residual gas is measured after the reaction is finished, the fluorine content in the fluorine-nitrogen mixed gas is tested according to the change of the volume before and after entering the absorption device, and the result can be directly and automatically calculated.
Description
Technical Field
The invention belongs to the technical field of gas analysis, and particularly relates to a method for automatically testing the fluorine content in a fluorine-nitrogen mixed gas.
Background
Fluorine gas is a very corrosive light yellow diatomic gas, has a strong pungent odor, is also a strong oxidant, and can be combined with almost all elements at normal temperature to generate a large amount of heat energy.
At present, fluorine gas obtained by electrolyzing anhydrous hydrogen fluoride and performing purification process treatment is used for preparing fluorides such as uranium hexafluoride, sulfur hexafluoride, boron trifluoride, silver difluoride, cobalt trifluoride, magnesium trifluoride and the like, and can also be used in the fields of laser gas or plastic fluorination treatment and the like. The fluorine-nitrogen mixed gas is a general name of a fluorine gas and nitrogen gas mixture with the fluorine gas content of less than 20% by volume, is used for cleaning a cavity of chip equipment in the field of electronic chip manufacturing, and has the fluorine gas purity of more than 99.9%; the fluorine plastic is used for end group treatment of fluorine-containing plastics such as PFA, PTFE, FEP and the like, surface fluorination of high molecular plastics and the like in the fluorine plastic industry, particularly the electronic industry.
The control of the fluorine gas concentration in the above process has an instructive effect on the above process, and therefore, the detection of fluorine gas is of great importance in the production.
At present, in the national standard GB/T26251 mixed gas of fluorine and nitrogen, F2 is converted into chlorine, and then the chlorine is tested by a gas chromatograph, the method has the defects that the conversion efficiency is not high, the chlorine is a highly toxic substance and can cause damage to the environment and human bodies, the residual F2 can seriously corrode equipment, the service life of the instrument is short, and the like. Therefore, the device for measuring the fluorine gas content in the fluorine-nitrogen mixed gas is provided to solve the problems.
In the patent 202111075708, X, a conversion pile is adopted to convert fluorine gas into oxygen gas through reaction, and then oxygen content is tested by using an oxygen content analysis device, so that the fluorine content in original sample gas is indirectly obtained, the analysis result can be directly read, complex calculation and pretreatment measures on the fluorine gas are avoided, and the operation is simple. The fluorine content in the fluorine-containing laser gas is tested, and Na2O2 is used as a filler in the conversion pile, so that the conversion pile has the defects of poor stability and unstable measurement data.
Patent 202111001790.1 is to present detection mode all arrive the workshop in advance and gather, send into corresponding laboratory after the end and carry out the chemical examination and detect, both delayed time, influence production again, greatly increased the cost of detection and work in good time, for this reason, proposed a device of fluorine gas content in measuring fluorine-containing mixed gas. However, the device needs to be subjected to separation by a three-stage chromatographic column and then is used for testing the fluorine gas content, and the device is complex in structure and large in error.
Patent 201711479720.0 discloses a fluorine gas analysis conversion device, belongs to fluorine gas content measurement technical field. The device absorbs fluorine gas through fine granular active metal oxides and finally generates oxygen gas, the fluorine gas enters from the bottom of the reaction tank, the fluorine gas can be fully absorbed in the active metal oxide layer with long stroke and long retention time, the conversion rate can reach 99% within 1min, and the determination result is accurate; the gas product after reaction only contains oxygen, and corrosion prevention treatment is not needed to be carried out on pipelines and equipment, so that the maintenance cost is low; whether the active metal oxide needs to be replaced or not is judged through color change in the indicator, and the method is more visual and rapid. However, this apparatus has a complicated structure and a high test cost, and it is difficult to satisfy the test of the fluorine gas content in the fluorine-containing gas having a high fluorine gas content.
Disclosure of Invention
The present invention is directed to provide an automatic measuring device for measuring the fluorine content in a mixed gas of fluorine and nitrogen, which solves the above-mentioned problems of the prior art.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
in one aspect, the invention discloses a device for measuring the content of fluorine in a fluorine-nitrogen mixed gas, which comprises
An air supply device: used for outputting the fluorine-nitrogen mixed gas and the purge gas of the purge device.
A metering device: for measuring the pressure before and after entering the adsorption device.
An adsorption device: the adsorption device is formed by connecting two adsorption towers with built-in fillers in parallel through pipelines. The packing which can react with the fluorine gas is filled inside the adsorption tower, and is used for fully reacting the fluorine gas entering the adsorption tower.
A vacuum device: for replacement of the entire device.
The invention has the following beneficial effects:
firstly, the method comprises the following steps: the fluorine gas in the fluorine-nitrogen gas for analysis is absorbed, so that the damage of the fluorine gas to human bodies is avoided.
Secondly, the method comprises the following steps: the pressure before and after the reaction can be automatically calculated according to the analysis result, so that the pretreatment and the complex calculation of the fluorine gas are avoided.
Thirdly, the method comprises the following steps: the set of analysis device is simple in test operation, short in detection time, high in efficiency, capable of realizing automatic and continuous inspection, capable of reducing labor cost and production cost and high in practicability.
On the basis of the technology, the following improvements can be made:
preferably, the sample gas supply device enters the second bypass through a main pipeline which is provided with a regulating valve (RV-802) and a pneumatic valve (AV-2) in sequence.
By adopting the preferable scheme, the pressure intensity entering the main pipeline and the switch are controlled by the adjusting valve (RV-802) and the pneumatic valve (AV-2).
Preferably, the pressure of the main line entering the second bypass is accurately measured by a measuring device.
With the preferred solution described above, the metering device on the second bypass consists of the pressure sensor PI-801 and the pneumatic valve AV-3.
Preferably, the metering devices (the pressure sensor PI-801 and the pneumatic valve AV-3) of the second bypass are respectively communicated with the air inlets of the adsorption towers AB-1 and AB-2 through the pneumatic valve AV-4, the reducer union, the filter and the restricted orifice plate.
By adopting the preferable scheme, the flow rate of the fluorine nitrogen entering the adsorption tower is controlled by adopting the pneumatic valve AV-4 and the flow-limiting orifice plate, so that the fluorine nitrogen entering the adsorption tower can fully react.
As a preferable aspect, an air-operated valve is provided in the second bypass.
By adopting the preferable scheme, pneumatic valves BV-1 and BV-3 are adopted to control the on and off of the pipeline at the air inlet of the adsorption tower.
Preferably, the apparatus for testing the fluorine gas content in the fluorine-nitrogen mixed gas further comprises:
the purge gas of the purge device is communicated with the main pipeline through a first bypass which is sequentially provided with a regulating valve (RV-801) and a pneumatic valve (AV-1).
By adopting the preferable scheme, the replacement of the front pipeline and the rear pipeline of the analysis is realized by adopting the purge gas supply device.
Preferably, the air outlet of the adsorption tower AB-1 and the air outlet of the adsorption tower AB-2 are connected with the main pipeline through a third bypass of the reducer union and the pneumatic valve AV-5.
By adopting the preferred scheme, pneumatic valves BV-2 and BV-4 are adopted to respectively control the opening and closing of the air outlets of the adsorption towers AB-1 and AB-2.
Preferably, the third bypass is provided with a reducer union and a pneumatic valve for connecting the air outlets of the adsorption towers AB-1 and AB-2 to the main pipeline.
Preferably, a pressure sensor PI-801E and a pneumatic valve AV-9 are arranged on the fifth bypass.
The pressure measuring device is used for measuring the pressure of the main pipeline.
Preferably, the vacuum device is connected to the main line by means of a pneumatic valve AV-6.
By adopting the preferred scheme, the inlet of the vacuum device is connected with the main pipeline by a vacuum pump NP-1 through a pneumatic valve AV-11, a buffer tank VP-1 and a pneumatic valve AV-6.
By adopting the preferable scheme, the outlet of the vacuum pump is connected to the tail gas of the process unit.
With the preferred arrangement described above, the fourth bypass at the outlet of the buffer tank VP-1 is connected to the process off-gas via a pneumatic valve AV-7.
By adopting the preferred scheme, the buffer tank VP-1 prevents oil and water from entering the main pipeline.
By adopting the preferable scheme, the tail gas generated by the device is treated, and the environmental pollution is avoided.
In a second aspect, the method for automatically testing the fluorine content in the fluorine-nitrogen mixed gas specifically comprises the following steps:
s1, confirming the airtightness of the device.
And S2, starting a vacuum pump and confirming the vacuum of the pipeline.
S3, replacement of the whole device.
And S4, confirming the pressure of the sample to be detected.
And S5, sucking the mixed gas into the adsorption tower for full reaction.
And S6, reading the gas pressure after the measurement is finished.
S7, replacement of the pipeline after the measurement is completed.
And S8, maintaining the pressure of the whole device.
S9, obtaining the fluorine gas content in the fluorine-nitrogen mixed gas by the percentage of the pressure difference before and after the reaction to the total pressure.
Compared with the prior art, the invention has the following advantages
The device lets in absorbing device including the fluorine nitrogen gas mixture of air feeder output and reacts, directly calculates fluorine content in the fluorine nitrogen gas mixture according to the change of getting into absorbing device front and back volume, avoids the not high and chlorine of national standard GB/T26251 "fluorine and fluorine nitrogen gas mixture" transfer efficiency to produce the injury for highly toxic substance meeting environment and human body, and remaining F2 can seriously corrode equipment, leads to shortcomings such as instrument life is lower.
The method has the advantages of simple device structure, low investment and capability of realizing automation of operation and continuity of test; the method is safe, environment-friendly and pollution-free, and is simple to operate; the method has the advantages of high conversion efficiency, high test precision and the like.
Drawings
FIG. 1 is a schematic diagram of an automatic testing device for fluorine content in a fluorine-containing mixed gas.
In the figure: 1-main, 2-first, 3-second, 4-third, 5-fourth, 6-fifth
RV-801-nitrogen pressure regulating valve, AV-1 nitrogen pneumatic valve, RV-802-fluorine nitrogen mixture pressure regulating valve, AV-2 fluorine nitrogen mixture pneumatic valve, AV-3-pneumatic valve, PI-801F-pressure sensor, AV-3-pneumatic valve, AV-4-pneumatic valve, AB-1-adsorption tower 1, AB-2-adsorption tower 2, AV-5-pneumatic valve, AV-2-pneumatic valve, PI-801E-pressure sensor, AV-9-pneumatic valve, AV-6-pneumatic valve, VP-1-surge tank, AV-8-pneumatic valve, NP-1-vacuum pump, AV-7-pneumatic valve, AV-11 pneumatic valve.
Detailed Description
The technical solution in the embodiment of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiment of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In order to achieve the purpose of the present invention, in some embodiments of an automatic testing device for fluorine content in a fluorine-containing mixed gas, as shown in fig. 1, the device comprises a gas supply device, a metering device and an adsorption device, wherein a vacuum device is communicated in sequence through a pipeline provided with a pneumatic valve.
The gas supply device is used for outputting fluorine-nitrogen mixed gas and device purge gas; the metering device is used for displaying the pressure before and after entering the adsorption device, the adsorption device is used for completely reacting fluorine gas in the fluorine-nitrogen mixed gas, and the vacuum device is used for providing the overall vacuum degree of the device.
The invention adopts the adsorption device to completely absorb the fluorine gas in the fluorine-nitrogen mixed gas, and obtains the fluorine content in the original mixed gas by utilizing the pressure change before and after entering the adsorption device.
The packing of the adsorption tower can be, but is not limited to, granular calcium oxide, and other materials capable of completely reacting fluorine gas are also possible. It is noteworthy that the packing within the adsorption column does not react with and generate other gases other than fluorine.
The invention has the following beneficial effects:
fluorine gas is completely absorbed, and residual gas enters process tail gas through a vacuum pump to be subjected to centralized treatment, so that the damage of the fluorine gas to a human body is avoided.
Secondly, after the reaction is finished, the analysis result is directly read. And the complex calculation and the pretreatment of the fluorine gas are avoided.
In order to further optimize the implementation effect of the invention, in other embodiments, the rest characteristics are the same, except that the sample gas supply device is communicated with the gas inlet of the adsorption tower through a second bypass by sequentially arranging pressure regulating valves RV-802 and AV-2.
With the adoption of the embodiment, the following beneficial effects are achieved: the pressure entering the second bypass and the switch are regulated and controlled by pressure regulating valves RV-802 and AV-2.
Further, on the basis of the implementation, the air outlet of the main pipeline is connected with the inlet of the adsorption device of the second bypass through the metering device and the flow-limiting orifice plate.
With the adoption of the embodiment, the following beneficial effects are achieved: the pressure sensor PI-801 is adopted to measure the gas pressure of the adsorption tower AB-1\ AB-2 entering the adsorption device in real time.
With the adoption of the embodiment, the following beneficial effects are achieved: the flow rate of gas entering an adsorption tower AB-1\ AB-2 of the adsorption device is controlled by adopting a flow-limiting orifice plate, so that the effectiveness of subsequent analysis of the fluorine-nitrogen mixed gas device is ensured.
Further, the main pipeline is connected to the adsorption tower pipeline through a second bypass on the basis of the above embodiment.
Further, in addition to the above embodiment, the second bypass is provided with pneumatic valves BV-1 and BV-3.
With the adoption of the embodiment, the following beneficial effects are achieved: pneumatic valves BV-1 and BV-3 are adopted to control the opening and closing of pipelines at the air inlet of the adsorption tower AB-1\ AB-2.
Further, in addition to the above implementation, the apparatus for measuring the content of fluorine in the mixed gas of fluorine and nitrogen further includes:
the purge gas from the gas supply (pipeline gas from the process) is communicated with the main pipeline through the first bypass of the pressure regulating valves RV-801 and AV-1.
With the adoption of the embodiment, the following beneficial effects are achieved: purging and replacement of the front and back lines of the analysis is achieved using a purge gas supply (duct gas from the process).
Further, on the basis of the implementation of the above, the air outlets of the adsorption towers are connected through a third bypass of BV-2, BV-4 and AV-5.
With the adoption of the embodiment, the following beneficial effects are achieved: BV-2 and BV-4 are adopted to control the opening and closing of pipelines at the gas outlet of the adsorption tower AB-1\ AB-2 of the adsorption device.
With the adoption of the embodiment, the following beneficial effects are achieved: AV-5 is adopted to control the on and off of the adsorption tower AB-1\ AB-2 of the adsorption device to the main pipeline.
In order to further optimize the implementation effect of the invention, in other embodiments, the rest characteristics are the same, except that the device for testing the content of fluorine in the fluorine-containing mixed gas further comprises;
the tail gas treatment device is characterized in that tail gas generated by the device is pumped to process tail gas by a vacuum device for unified treatment.
The inlet of the vacuum device consists of a vacuum pump NP-1, an AV-11 and a buffer tank VP-1.
The vacuum device is connected to the main line by means of a pneumatic valve AV-6.
The outlet is connected to the process tail gas for uniform treatment.
The embodiment has the following beneficial effects: the fourth bypass at the outlet of the buffer tank VP-1 is connected to the process off-gas via a pneumatic valve AV-7.
The embodiment has the following beneficial effects: the buffer tank VP-1 prevents oil and water from entering the main pipeline.
The embodiment has the following beneficial effects: the tail gas is treated to avoid environmental pollution.
The invention also discloses a method for testing the content of fluorine in the fluorine-containing mixed gas, which is used for testing by using the device for testing the content of fluorine in the fluorine-containing mixed gas disclosed by any one of the examples and specifically comprises the following steps:
the fluorine-nitrogen mixed gas output by the sample gas supply device is completely absorbed by the fluorine gas in the adsorption tower, and the content of the fluorine gas is obtained by utilizing the pressure change before and after the fluorine gas enters the adsorption tower AB-1\ AB-2.
Further, in some embodiments, a purge gas supply is used to purge all of the lines prior to testing. Before the analysis, the air in the pipeline is replaced completely, and the accuracy and effectiveness of the analysis are improved.
In order to provide a more complete understanding of the present invention, specific examples are set forth below. It should be noted that the specific embodiments are only related to certain embodiments of the present invention, and do not limit the protection scope of the present invention.
Example 1:
as shown in fig. 1, the test apparatus includes: air feeder, metering device, adsorption equipment, vacuum device.
The sample is purchased externally 20% volF 2 The mixed gas of (1).
The gas supply device comprises a purge gas device and a sample gas supply device.
The purge gas device is arranged on the first bypass through a pressure regulating valve RV-801 and an air-operated valve AV-1, and the sample gas supply device pressure regulating valve RV-802 and the air-operated valve AV-2 are arranged on the main pipeline.
The metering device consists of a pressure sensor PI-801 and a pneumatic valve AV-4 and is arranged on the second bypass.
The adsorption device is formed by connecting an adsorption tower AB-1 and an adsorption tower AB-2 in parallel, an inlet is arranged on the second bypass, and an outlet is arranged on the third bypass.
The vacuum device consists of a vacuum pump NP-1, a pneumatic valve AV-11 and a buffer tank VP-1; connected to the main line by means of a pneumatic valve AV-6.
To prevent leakage, VCR connections are used between the valves and EP 316 tubes are used to avoid corrosion of the clean lines.
The fillers in the adsorption towers AB-1 and AB-2 are granular calcium oxide.
The principle on which the invention is based is as follows: the fluorine gas reacts with the absorption tower packing calcium oxide to generate calcium fluoride and oxygen, and the content of the fluorine gas is indirectly obtained by measuring the pressure change before and after the reaction. The reaction formula is as follows: 2F 2 +2CaO＝2CaF 2 +O 2 Conversion of fluorine to O 2 The number of moles of gas is reduced from 2 to 1, and F can be calculated from the formula PV ═ nRT 2 Content in the mixed gas.
The adsorption towers AB-1 and AB-2 are cylindrical and made of 316 materials and have the size
The fluorine gas reacts with calcium oxide to generate calcium fluoride, the calcium fluoride is white powder, and when the temperature of the buffer tank is abnormal (exceeds 34 ℃), the adsorption towers AB-1 to AB-2 are switched. The adsorption tower AB-1 is converted by adopting new filler for standby.
The purge gas used was nitrogen with a purity of 99.999%.
And pumping the tail gas to process tail gas through a vacuum device for unified treatment.
The filter adopts the filter core of 0.1um, avoids calcium oxide, calcium fluoride powder to get into the rear end and causes the filling of valve to influence normal analysis.
The flow-limiting orifice plate adopts 100micro and is made of corrosion-resistant materials.
The pneumatic valves AV-1, AV-2, AV-3, AV-4, AV-5, AV-7, AV-8 and AV-9 adopt diaphragm valves.
Example 2
Test gas is configured 15% volF 2 The same as in example 1.
Example 3
Test gas is 5% volF 2 The same as in example 1.
Example 4
The specific test method is as follows:
s1 confirmation of device airtightness:
opening AV-5, BV-2, BV-1 (or BV-3, BV-4), AV-4, AV-10 and AV-1; the pressure regulating valve RV-801 to PI-801F is adjusted to 0.1 +/-0.005 MPa, and the pressure is unchanged in 10 min.
S2, starting a vacuum pump, confirming pipeline vacuum:
starting a vacuum pump, turning on AV-6 to PI-801E to-0.1000 MPa, and then turning off AV-6.
S3, replacement of device:
opening AV-5, BV-2, BV-1 (or BV-3, BV-4), AV-4, AV-10 and AV-1; regulating the pressure regulating valve RV-801 to PI-801F to 0.1 +/-0.005 MPa, and then closing AV-1; AV-6 was turned on to PI-801E to-0.1000 MPa and then turned off (repeated 3 times). And finally confirming PI-801E to-0.1000 MPa, and turning off BV-2 and AV-5.
S4, confirming the pressure of the sample to be detected:
opening AV-2 and AV-4 to adjust the pressure regulating valve RV-802 to PI-801F to 0MPa
S5, sucking the mixed gas into an adsorption tower for full reaction:
and (3) opening the BV-1 slowly, and allowing the mixed gas to enter an adsorption tower for reaction for 10 min.
S6, reading the gas pressure after the measurement:
after 10min, reading the reading of PI-801F as V, reading every 2min, and recording the numerical value when the reading of PI-801F is not changed after reading twice continuously.
The following formula for the analytical results:
F 2 ％＝[(-2V)/0.1]*100
in the formula: v-reading of PI-801E after the reaction has ended (negative pressure)
S7, replacement of line after completion of measurement:
regulating the pressure regulating valve RV-801 to PI-801F to 0.1 +/-0.005 MPa, and then closing the AV-1; turning on AV-6, AV-7 to PI-801E to 0.0MPA and then turning off AV-7 (repeating for 10 times); opening AV-10, vacuumizing for 2min, and closing AV-10.
S8, integral pressure maintaining of the device:
and (4) regulating the pressure regulating valves RV-801 to PI-801F to 0.1 +/-0.005 MPa, and then closing AV-1. And closing AV-6, AV-5, BV-2, BV-1 (or BV-3 and BV-4), AV-4 and AV-1 in sequence from back to front.
S9, obtaining the fluorine gas content in the fluorine-nitrogen mixed gas by the percentage of the pressure difference before and after the reaction to the total pressure.
The analysis is finished.
Note that: when the two steps of S1 and S2 are carried out, whether leakage points exist at the joints of pipelines and valves can be effectively detected, if leakage exists, the two steps of S1 and S2 are required to be implemented after leakage elimination so as to ensure no leakage. The device and the method for testing the fluorine content in the fluorine-nitrogen mixed gas can also be used for testing the fluorine content of the fluorine-containing laser gas (the commonly used fluorine gas is prepared to have the content of about 0.1-0.5%, and other residual gases comprise neon, argon, helium, krypton and the like).
According to the technical scheme, 4 samples are selected to carry out method repeatability tests so as to verify the precision of the measuring device.
The results obtained are shown in table 1 below.
Table 1: precision test result of fluorine content in sample (n ═ 6)
As can be seen from Table 1, the relative standard deviation is less than or equal to 10%, which shows that the method has better precision.
In order to verify the accuracy of the technical scheme, the recovery test is adopted for further verification, the recovery test adopts the step of adding a fluorine-containing mixture with a known concentration, and according to the experimental conditions, the fluorine-containing mixed gas with different contents is added into the device after the determination is finished for standard addition recovery, and the obtained results are shown in table 2.
TABLE 2
| Sample number | Measurement value (%) | Plus amount (%) | Recovery (%) |
| Example 1 | 20.03 | 20 | 99.83 |
| Example 2 | 15.30 | 15 | 98.04 |
| Example 3 | 5.13 | 5 | 97.40 |
| Example 4 | 2.06 | 2 | 97.21 |
As can be seen from Table 2, the recovery rate is 90-110%, which indicates that the method is accurate and reliable.
The above embodiments are merely illustrative of the technical concept and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the content of the present invention and implement the present invention, and not to limit the scope of the present invention, and all equivalent changes or modifications made according to the spirit of the present invention should be covered by the scope of the present invention.
Claims (9)
1. A method for automatically testing the fluorine content in a fluorine-nitrogen mixed gas is characterized by comprising the following steps: the device comprises a gas supply device, a metering device, an adsorption device and a vacuum device.
2. The method for automatically testing the fluorine content in the fluorine-nitrogen mixed gas according to claim 1, wherein the method comprises the following steps:
the gas supply device consists of a pressure reducing valve and a control valve and is used for outputting fluorine-nitrogen mixed gas, nitrogen and purge gas for purging;
a metering device: the device comprises a control valve, a pressure sensor and the like; the metering of gas before and after reaction;
an adsorption device: consists of a control valve, an adsorption tower and the like; the adsorption device consists of two adsorption towers which are connected in parallel; the absorption tower is internally provided with reaction filler for fully reacting fluorine gas in the fluorine-nitrogen mixed gas;
a vacuum device: the device consists of a vacuum pump, a buffer tank, a pressure sensor, a control valve and the like, and is used for replacing the whole device.
3. The method for automatically testing the fluorine content in the fluorine-nitrogen mixed gas according to claim 1, wherein the method comprises the following steps: the air supply device, the metering device, the adsorption device and the vacuum device are sequentially communicated through a pipeline provided with a control valve.
4. The method for automatically testing the fluorine content in the fluorine-nitrogen mixed gas according to claim 1, wherein the method comprises the following steps: the fluorine nitrogen gas from the process of the gas supply device is communicated with the vacuum device through a main pipeline which is sequentially provided with a regulating valve and a pneumatic valve, and the sweeping gas for the sweeping device is communicated with the main pipeline through a first bypass which is sequentially provided with the regulating valve and the pneumatic valve.
5. The method for automatically testing the fluorine content in the fluorine-nitrogen mixed gas according to claim 1, wherein the method comprises the following steps: the metering device is composed of a pressure sensor from the second bypass and a pneumatic valve and is connected with the main pipeline through a pipeline; the reducing joint and the filter are communicated with the adsorption device through a pneumatic valve.
6. The method for automatically testing the fluorine content in the fluorine-nitrogen mixed gas according to claim 1, wherein the method comprises the following steps: the adsorption device is formed by connecting two adsorption towers with built-in fillers in parallel through pipelines; an inlet of the adsorption tower 1 is connected with a second bypass through a pneumatic valve; the outlet is communicated with the main pipeline through a pneumatic valve after being connected with the third bypass, and the inlet of the adsorption tower 2 is connected with the second bypass through the pneumatic valve; the outlet is communicated with the main pipeline through a pneumatic valve after being connected with the third bypass.
7. The method for automatically testing the fluorine content in the fluorine-nitrogen mixed gas according to claim 1, wherein the method comprises the following steps: the inlet of the vacuum device is connected with a main pipeline through a vacuum pump, a pneumatic valve, a buffer tank and a pneumatic valve, the outlet of the vacuum device is connected to the tail gas of the process device, and the outlet of the buffer tank can also be connected to the tail gas of the process device through a fourth bypass and the pneumatic valve.
8. The method for automatically testing the fluorine content in the fluorine-nitrogen mixture gas as claimed in claims 1 to 7, wherein: the testing device for testing the content of the fluorine in the fluorine-nitrogen mixed gas is utilized to test, and the specific content comprises the following contents: and (3) introducing the fluorine-nitrogen mixed gas output by the gas supply device into an adsorption tower through a metering device, reacting fluorine gas in the adsorption tower, not reacting nitrogen gas, and obtaining the fluorine gas content in the fluorine-nitrogen mixed gas by utilizing the percentage of the pressure difference before and after the reaction to the total pressure.
9. The method for automatically testing the fluorine content in the fluorine-nitrogen mixture gas as claimed in claim 8, wherein: before testing, all lines were purged using a purge gas supply.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| IT8919907A0 (en) * | 1988-03-31 | 1989-03-24 | Central Glass Co Ltd | METHOD AND DEVICE FOR ANALYZING GASES CONTAINING FLUORINE. |
| CN101013112A (en) * | 2006-11-01 | 2007-08-08 | 石平湘 | Detecting method of drop fluorine in quasi-molecule laser gas |
| CN108287157A (en) * | 2017-12-29 | 2018-07-17 | 和立气体（上海）有限公司 | A kind of fluorine gas analysis reforming unit |
| CN113917075A (en) * | 2021-09-14 | 2022-01-11 | 苏州金宏气体股份有限公司 | Device and method for testing fluorine content in fluorine-containing mixed gas |
-
2022
- 2022-04-18 CN CN202210403378.0A patent/CN114813448A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| IT8919907A0 (en) * | 1988-03-31 | 1989-03-24 | Central Glass Co Ltd | METHOD AND DEVICE FOR ANALYZING GASES CONTAINING FLUORINE. |
| CN101013112A (en) * | 2006-11-01 | 2007-08-08 | 石平湘 | Detecting method of drop fluorine in quasi-molecule laser gas |
| CN108287157A (en) * | 2017-12-29 | 2018-07-17 | 和立气体（上海）有限公司 | A kind of fluorine gas analysis reforming unit |
| CN113917075A (en) * | 2021-09-14 | 2022-01-11 | 苏州金宏气体股份有限公司 | Device and method for testing fluorine content in fluorine-containing mixed gas |
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