CN111983084A - Method for detecting content of hydrolysable fluoride in sulfur hexafluoride gas - Google Patents
Method for detecting content of hydrolysable fluoride in sulfur hexafluoride gas Download PDFInfo
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- CN111983084A CN111983084A CN202010844898.6A CN202010844898A CN111983084A CN 111983084 A CN111983084 A CN 111983084A CN 202010844898 A CN202010844898 A CN 202010844898A CN 111983084 A CN111983084 A CN 111983084A
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- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 title claims abstract description 58
- 229910018503 SF6 Inorganic materials 0.000 title claims abstract description 57
- 229960000909 sulfur hexafluoride Drugs 0.000 title claims abstract description 57
- SFZCNBIFKDRMGX-UHFFFAOYSA-N sulfur hexafluoride Chemical compound FS(F)(F)(F)(F)F SFZCNBIFKDRMGX-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 238000000034 method Methods 0.000 title claims abstract description 33
- 239000011521 glass Substances 0.000 claims abstract description 26
- 238000010521 absorption reaction Methods 0.000 claims abstract description 23
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims abstract description 22
- 239000000243 solution Substances 0.000 claims abstract description 22
- -1 fluorine ions Chemical class 0.000 claims abstract description 18
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 14
- 239000011737 fluorine Substances 0.000 claims abstract description 14
- 238000012360 testing method Methods 0.000 claims abstract description 13
- 239000007788 liquid Substances 0.000 claims abstract description 12
- 239000011775 sodium fluoride Substances 0.000 claims abstract description 11
- 235000013024 sodium fluoride Nutrition 0.000 claims abstract description 11
- 239000008367 deionised water Substances 0.000 claims abstract description 9
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 9
- 150000002500 ions Chemical class 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 16
- 239000007864 aqueous solution Substances 0.000 claims description 11
- 238000005406 washing Methods 0.000 claims description 8
- 239000006096 absorbing agent Substances 0.000 claims description 4
- 239000008139 complexing agent Substances 0.000 abstract description 7
- 229910052746 lanthanum Inorganic materials 0.000 abstract description 3
- 239000012086 standard solution Substances 0.000 abstract description 2
- 238000011010 flushing procedure Methods 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000003513 alkali Substances 0.000 description 2
- 238000004737 colorimetric analysis Methods 0.000 description 2
- 239000011810 insulating material Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 2
- 229910052753 mercury Inorganic materials 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 230000006641 stabilisation Effects 0.000 description 2
- 238000011105 stabilization Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 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
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/14—Preparation by elimination of some components
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/86—Signal analysis
- G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
- G01N30/8679—Target compound analysis, i.e. whereby a limited number of peaks is analysed
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N2030/042—Standards
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/14—Preparation by elimination of some components
- G01N2030/143—Preparation by elimination of some components selective absorption
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Abstract
A method for detecting the content of hydrolyzable fluoride in sulfur hexafluoride gas relates to a method for detecting components in sulfur hexafluoride gas. The invention aims to solve the technical problems that the prior method for measuring the content of the hydrolyzable fluoride in the sulfur hexafluoride gas needs to control pH or has short shelf life of a complexing agent and needs to be checked frequently. The absorption liquid and the flushing liquid in the glass absorption bottle are transferred into a volumetric flask together, and are diluted to a scale by deionized water to be used as a solution to be measured; preparing known sodium fluoride standard solutions with different concentrations, drawing a standard curve of fluorine ions by using an ion chromatograph, testing the concentration of the fluorine ions in the solution to be tested, and calculating the mass fraction of hydrolyzable fluoride contained in sulfur hexafluoride gas. The invention can provide a new method for detecting the content of hydrolysable fluoride in sulfur hexafluoride gas. The method does not need to strictly control the pH value of the solution to be 5.0-5.5, does not need to frequently observe the stable condition of the alizarin-lanthanum complexing agent, and has simpler operation and strong practicability.
Description
Technical Field
The invention relates to a method for detecting components in sulfur hexafluoride gas.
Background
The hydrolysable fluoride in the sulfur hexafluoride gas is one of important indexes for controlling the quality of the sulfur hexafluoride gas, not only can corrode equipment and solid insulating materials and accelerate the degradation of the equipment and the solid insulating materials, but also the content of the hydrolysable fluoride represents the toxicity to a certain extent.
The method for determining the content of hydrolyzable fluoride in sulfur hexafluoride gas is specified in Standard DL/T918-2005 hydrolyzable fluoride content determination in Sulfur hexafluoride gas, which is two: colorimetric methods and fluoride ion selective electrode methods. When the fluorine ion content is measured by the fluorine ion selective electrode method, the pH value of the solution must be strictly controlled within 5.0-5.5, because when the pH values of the solutions are different, the measured negative potential values of the samples are different, and the time required for reaching equilibrium (the difference of the negative potential values is not more than 1 within 1 min) is different. When the pH value is 5.0-5.5, the difference between the initial negative potential value and the final negative potential value is minimum, and the time for reaching the balance is shortest; when the pH value is less than 5.0 and greater than 6.0, the equilibrium time is longer, and the difference between the initial negative potential value and the final negative potential value is large, so that the error of the measurement result is increased. When a standard solution of a working curve is prepared in a colorimetric method, the pH value is not adjusted, the analysis time is greatly shortened, and chemical reagents are saved, but the alizarin-lanthanum complexing agent has a one-week stabilization period at room temperature, can be stored for one month in a refrigerator, so that the state of the complexing agent needs to be checked frequently, and the measurement result is influenced if the stabilization condition of the complexing agent is not observed in time.
Disclosure of Invention
The invention provides a method for detecting the content of hydrolyzable fluoride in sulfur hexafluoride gas, aiming at solving the technical problems that the existing method for determining the content of hydrolyzable fluoride in sulfur hexafluoride gas needs to control pH or the quality guarantee period of a complexing agent is short, and the content needs to be frequently checked.
The method for detecting the content of the hydrolysable fluoride in the sulfur hexafluoride gas is carried out according to the following steps:
respectively preparing sodium fluoride aqueous solutions with different concentrations, and respectively testing the sodium fluoride aqueous solutions with different concentrations by using an ion chromatograph to obtain a fluorine ion standard curve; the physical quantity of the ordinate of the fluorine ion standard curve is the concentration of fluorine ions, and the unit is mu g/L; the physical quantity of the abscissa of the standard curve of fluoride ions is the peak area in μ S min;
absorbing sulfur hexafluoride gas to be detected by adopting a method in 5.2.1-5.2.4 in standard DL/T918-2005 'determination method of content of hydrolyzable fluoride in sulfur hexafluoride gas'; transferring all liquid in the glass absorption bottle into a 100mL volumetric flask, washing the inner container of the glass absorption bottle with deionized water, transferring the washing liquid into the 100mL volumetric flask, and adding the deionized water into the 100mL volumetric flask to scale to obtain a solution to be detected;
thirdly, testing the peak area of the solution to be tested prepared in the second step by using an ion chromatograph, and obtaining the corresponding fluorine ion concentration a through the fluorine ion standard curve drawn in the first step, namely the concentration of the fluorine ions in the solution to be tested;
the content of hydrolyzable fluoride in sulfur hexafluoride gas is expressed by the mass ratio of hydrofluoric acid;
by the following formula
The content of hydrolyzable fluoride in the sulfur hexafluoride gas can be calculated;
in the formula:
WHFthe mass ratio of hydrofluoric acid is the content of hydrolysable fluoride in sulfur hexafluoride gas, and the unit is mu g/g;
a-the concentration of the fluorine ions in the solution to be detected, wherein the unit is mu g/L;
v-the volume of the glass absorber, in L;
p-atmospheric pressure, in Pa;
t-ambient temperature in units of;
6.16-Sulfur hexafluoride gas density in g/L.
The method is a novel method for detecting the content of the hydrolysable fluoride in the sulfur hexafluoride gas, does not need to strictly control the pH value of the solution to be 5.0-5.5, does not need to frequently observe the stability of the alizarin-lanthanum complexing agent, and is simpler to operate and strong in practicability.
Drawings
FIG. 1 is a schematic diagram of a device for absorbing sulfur hexafluoride gas to be detected in a first test, wherein 1 is a glass absorption bottle, 2 and 3 are vacuum three-way pistons, 4 is a U-shaped mercury differential pressure gauge, 5 is a bladder, 6 is a medical injector, 7 is an upper branch pipe, and 8 is a spiral clamp;
fig. 2 is a plot of the fluoride ion standard obtained in step one of experiment one.
Detailed Description
The first embodiment is as follows: the embodiment is a method for detecting the content of hydrolyzable fluoride in sulfur hexafluoride gas, which is specifically carried out according to the following steps:
respectively preparing sodium fluoride aqueous solutions with different concentrations, and respectively testing the sodium fluoride aqueous solutions with different concentrations by using an ion chromatograph to obtain a fluorine ion standard curve; the physical quantity of the ordinate of the fluorine ion standard curve is the concentration of fluorine ions, and the unit is mu g/L; the physical quantity of the abscissa of the standard curve of fluoride ions is the peak area in μ S min;
absorbing sulfur hexafluoride gas to be detected by adopting a method in 5.2.1-5.2.4 in standard DL/T918-2005 'determination method of content of hydrolyzable fluoride in sulfur hexafluoride gas'; transferring all liquid in the glass absorption bottle into a 100mL volumetric flask, washing the inner container of the glass absorption bottle with deionized water, transferring the washing liquid into the 100mL volumetric flask, and adding the deionized water into the 100mL volumetric flask to scale to obtain a solution to be detected;
thirdly, testing the peak area of the solution to be tested prepared in the second step by using an ion chromatograph, and obtaining the corresponding fluorine ion concentration a through the fluorine ion standard curve drawn in the first step, namely the concentration of the fluorine ions in the solution to be tested;
the content of hydrolyzable fluoride in sulfur hexafluoride gas is expressed by the mass ratio of hydrofluoric acid;
by the following formula
The content of hydrolyzable fluoride in the sulfur hexafluoride gas can be calculated;
in the formula:
WHFthe mass ratio of hydrofluoric acid is the content of hydrolysable fluoride in sulfur hexafluoride gas, and the unit is mu g/g;
a-the concentration of the fluorine ions in the solution to be detected, wherein the unit is mu g/L;
v-the volume of the glass absorber, in L;
p-atmospheric pressure, in Pa;
t-ambient temperature in units of;
6.16-Sulfur hexafluoride gas density in g/L.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: aqueous solutions of sodium fluoride at concentrations of 2.1. mu.g/L, 3.3. mu.g/L, 4.8. mu.g/L, 7.3. mu.g/L and 10.1. mu.g/L were prepared, respectively. The rest is the same as the first embodiment.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: and the glass absorption bottle in the step two is a conical bottle. The others are the same as in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment mode and one of the first to third embodiment modes is: and the volume of the glass absorption bottle in the step two is 1000 mL. The rest is the same as one of the first to third embodiments.
The fifth concrete implementation mode: the fourth difference between this embodiment and the specific embodiment is that: and the volume of the glass absorption bottle in the step two is 800 mL. The rest is the same as the fourth embodiment.
The invention was verified with the following tests:
test one: the test is a method for detecting the content of hydrolyzable fluoride in sulfur hexafluoride gas, and is specifically carried out according to the following steps:
firstly, respectively preparing sodium fluoride aqueous solutions with the concentrations of 2.1 mu g/L, 3.3 mu g/L, 4.8 mu g/L, 7.3 mu g/L and 10.1 mu g/L, and respectively testing the sodium fluoride aqueous solutions with different concentrations by using an ion chromatograph to obtain a fluorine ion standard curve (shown in figure 2); the physical quantity of the abscissa of the fluorine ion standard curve is the concentration of fluorine ions, and the unit is mu g/L; the physical quantity of the ordinate of the standard curve of fluoride ions is the peak area in μ S × min;
secondly, absorbing sulfur hexafluoride gas to be measured by adopting a method in 5.2.1 to 5.2.4 of a standard DL/T918-2005 hydrolyzable fluoride content determination method in sulfur hexafluoride gas, wherein the process is as follows, and is shown in figure 1:
1. extruding air in the bladder 5 completely, filling sulfur hexafluoride gas to be detected into the bladder 5, extruding the sulfur hexafluoride gas completely, filling the sulfur hexafluoride gas to be detected again, repeating the operation for three times to ensure that the bladder 5 is completely free of air and completely filled with the sulfur hexafluoride gas to be detected, and screwing the screw clamp 8;
2. installing a glass absorption bottle 1 with accurately measured volume in advance and a bladder 5 filled with sulfur hexafluoride gas to be measured according to the figure 1; respectively rotating the vacuum three-way pistons 2 and 3 to the positions a and b, and starting a vacuum pump to start vacuumizing; continuing to pump for 2min after the liquid level of the U-shaped mercury differential pressure gauge 4 is stable (the vacuum degree is 13.3 Pa), then rotating the vacuum piston 2 to the position b, disconnecting the connection part of the glass absorption bottle 1 and the vacuum system, and stopping pumping vacuum;
3. the spiral clamp 8 is slowly unscrewed, and sulfur hexafluoride gas in the bladder 5 is slowly filled in the glass absorption bottle 1; rotating the vacuum piston 2 to c moment and then rapidly rotating to b moment to balance the pressure in the glass absorption bottle 1 with the atmospheric pressure;
4. slowly injecting 10mL of sodium hydroxide aqueous solution (0.1mol/L) into the glass absorption bottle 1 from the rubber tube by using a medical injector 6 (at the moment, the ball bladder 5 filled with sulfur hexafluoride gas is slightly squeezed by hands so as to completely inject the alkali liquid), then screwing the vacuum piston 2 to the position d, screwing the spiral clamp 8, taking off the ball bladder 5, tightly holding the glass absorption bottle 1, and forcefully shaking for 1min every 5min within 1h (forcefully shaking is certainly needed so as to ensure that the sulfur hexafluoride gas is fully contacted with the dilute alkali as far as possible);
5. transferring all the liquid in the glass absorption bottle 1 into a 100mL volumetric flask, washing the inner container of the glass absorption bottle with deionized water, transferring the washing liquid into the 100mL volumetric flask, and adding deionized water into the 100mL volumetric flask to scale to obtain a solution to be detected;
thirdly, testing the peak area of the solution to be tested prepared in the second step by using an ion chromatograph, and obtaining the corresponding fluorine ion concentration a through the fluorine ion standard curve drawn in the first step, namely the concentration of the fluorine ions in the solution to be tested;
the content of hydrolyzable fluoride in sulfur hexafluoride gas is expressed by the mass ratio of hydrofluoric acid;
by the following formula
The content of hydrolyzable fluoride in the sulfur hexafluoride gas can be calculated;
in the formula:
WHFthe mass ratio of hydrofluoric acid is the content of hydrolysable fluoride in sulfur hexafluoride gas, and the unit is mu g/g;
a-the concentration of the fluorine ions in the solution to be detected, wherein the unit is mu g/L;
v-the volume of the glass absorber, in L;
p-atmospheric pressure, in Pa;
t-ambient temperature in units of;
6.16-Sulfur hexafluoride gas density in g/L.
Claims (5)
1. A method for detecting the content of hydrolyzable fluoride in sulfur hexafluoride gas is characterized in that the method for detecting the content of hydrolyzable fluoride in sulfur hexafluoride gas is carried out according to the following steps:
respectively preparing sodium fluoride aqueous solutions with different concentrations, and respectively testing the sodium fluoride aqueous solutions with different concentrations by using an ion chromatograph to obtain a fluorine ion standard curve; the physical quantity of the ordinate of the fluorine ion standard curve is the concentration of fluorine ions, and the unit is mu g/L; the physical quantity of the abscissa of the standard curve of fluoride ions is the peak area in μ S min;
absorbing sulfur hexafluoride gas to be detected by adopting a method in 5.2.1-5.2.4 in standard DL/T918-2005 'determination method of content of hydrolyzable fluoride in sulfur hexafluoride gas'; transferring all liquid in the glass absorption bottle into a 100mL volumetric flask, washing the inner container of the glass absorption bottle with deionized water, transferring the washing liquid into the 100mL volumetric flask, and adding the deionized water into the 100mL volumetric flask to scale to obtain a solution to be detected;
thirdly, testing the peak area of the solution to be tested prepared in the second step by using an ion chromatograph, and obtaining the corresponding fluorine ion concentration a through the fluorine ion standard curve drawn in the first step, namely the concentration of the fluorine ions in the solution to be tested;
the content of hydrolyzable fluoride in sulfur hexafluoride gas is expressed by the mass ratio of hydrofluoric acid;
by the following formula
The content of hydrolyzable fluoride in the sulfur hexafluoride gas can be calculated;
in the formula:
WHFthe mass ratio of hydrofluoric acid is the content of hydrolysable fluoride in sulfur hexafluoride gas, and the unit is mu g/g;
a-the concentration of the fluorine ions in the solution to be detected, wherein the unit is mu g/L;
v-the volume of the glass absorber, in L;
p-atmospheric pressure, in Pa;
t-ambient temperature in units of;
6.16-Sulfur hexafluoride gas density in g/L.
2. The method for detecting the content of hydrolyzable fluoride in sulfur hexafluoride gas as claimed in claim 1, wherein the aqueous solutions of sodium fluoride with concentrations of 2.1 μ g/L, 3.3 μ g/L, 4.8 μ g/L, 7.3 μ g/L and 10.1 μ g/L are prepared, respectively.
3. The method for detecting the content of hydrolyzable fluoride in sulfur hexafluoride gas as claimed in claim 1, wherein the glass absorption bottle in the second step is a conical bottle.
4. The method for detecting the content of hydrolyzable fluoride in sulfur hexafluoride gas as claimed in claim 1, wherein the volume of the glass absorption bottle in the second step is 1000 mL.
5. The method for detecting the content of hydrolyzable fluoride in sulfur hexafluoride gas as claimed in claim 1, wherein the volume of the glass absorption bottle in the second step is 800 mL.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2006078226A (en) * | 2004-09-07 | 2006-03-23 | Fuji Electric Holdings Co Ltd | Ion quantitative analyzing method and fluorine ion quantitative analyzing method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006078226A (en) * | 2004-09-07 | 2006-03-23 | Fuji Electric Holdings Co Ltd | Ion quantitative analyzing method and fluorine ion quantitative analyzing method |
Non-Patent Citations (2)
| Title |
|---|
| 中华人民共和国国家发展和改革委员会: "六氟化硫气体中可水解氟化物含量测定法", 《中华人民共和国电力行业标准DL/T 918-2005》 * |
| 邱妮 等: "离子色谱法检测可水解氟化物在SF6设备故障判定中的应用", 《高压电器》 * |
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Application publication date: 20201124 |