CN104807719A - Direct quantitative calibration method for measuring hydrolyzable fluoride in sulfur hexafluoride gas - Google Patents

Direct quantitative calibration method for measuring hydrolyzable fluoride in sulfur hexafluoride gas Download PDF

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CN104807719A
CN104807719A CN201510189593.5A CN201510189593A CN104807719A CN 104807719 A CN104807719 A CN 104807719A CN 201510189593 A CN201510189593 A CN 201510189593A CN 104807719 A CN104807719 A CN 104807719A
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gas
fluoride
sulfur hexafluoride
hydrolyzable
sof2
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CN104807719B (en
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朱洪斌
张晓琴
王晨
余翔
解文龙
张建国
陈大兵
刘建军
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ZHONGHUI INSTRUMENT CO Ltd
State Grid Corp of China SGCC
State Grid Jiangsu Electric Power Co Ltd
Electric Power Research Institute of State Grid Jiangsu Electric Power Co Ltd
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ZHONGHUI INSTRUMENT CO Ltd
State Grid Corp of China SGCC
State Grid Jiangsu Electric Power Co Ltd
Electric Power Research Institute of State Grid Jiangsu Electric Power Co Ltd
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Abstract

The invention discloses a direct quantitative calibration method for measuring hydrolyzable fluoride in sulfur hexafluoride gas, and belongs to the technical field of equipment detection. The direct quantitative calibration method for measuring hydrolyzable fluoride in sulfur hexafluoride gas comprises the following steps: taking easily hydrolyzable SOF2 standard gas as a quantitative reference, feeding the SOF2 standard gas into an absorbent solution, and completely dissolving the SOF2 standard gas in the absorbent solution, wherein the fluoride ion concentration of the absorbent solution is in direct proportion to the feeding volume of the SOF2 standard gas. According to the method, quantification of hydrolyzable fluoride in the sulfur hexafluoride gas directly traces to the source of national standard material, the difficulties that workload of hydrolyzable fluoride measuring experiment is large, the operation is complex, and the parallel test error is large are solved, the accuracy and stability of the experiment are ensured, and meanwhile, the efficiency of sulfur hexafluoride gas quality control is improved.

Description

六氟化硫气体中可水解氟化物测量的直接定量校验方法A Direct Quantitative Calibration Method for the Measurement of Hydrolyzable Fluoride in Sulfur Hexafluoride Gas

技术领域 technical field

本发明涉及一种六氟化硫气体中可水解氟化物测量的直接定量校验方法,属于设备检测技术领域。 The invention relates to a direct quantitative verification method for measuring hydrolyzable fluoride in sulfur hexafluoride gas, belonging to the technical field of equipment detection.

背景技术 Background technique

六氟化硫气体中可水解氟化物含量是控制气体质量的关键指标。目前可用于可水解氟化物测量的方法中,均需配制多个不同氟离子浓度的工作液,操作繁琐、工作量大。 The content of hydrolyzable fluoride in sulfur hexafluoride gas is a key indicator for controlling gas quality. Currently available methods for the measurement of hydrolyzable fluoride require the preparation of multiple working fluids with different fluoride ion concentrations, which is cumbersome and requires heavy workload.

发明内容 Contents of the invention

本发明的目的是提供一种六氟化硫气体中可水解氟化物测量的直接定量校验方法,采用标准气体的方法代替工作液来定量校验可水解氟化物的测量,解决现有技术中均需配制多个不同氟离子浓度的工作液,操作繁琐、工作量大的技术问题。 The purpose of the present invention is to provide a direct quantitative verification method for the measurement of hydrolyzable fluoride in sulfur hexafluoride gas, using the method of standard gas instead of working fluid to quantitatively verify the measurement of hydrolyzable fluoride, solving the problems in the prior art It is necessary to prepare multiple working solutions with different fluoride ion concentrations, which is a technical problem of cumbersome operation and heavy workload.

本发明采用如下技术方案:一种六氟化硫气体中可水解氟化物测量的直接定量校验方法,其特征在于,选取易水解的氟化亚硫酰(SOF2)标准气体作为定量的依据,将所述SOF2标准气体通入吸收溶液中,所述SOF2标准气体在所述吸收溶液中完全溶解,所述吸收溶液中的氟离子浓度与所述SOF2标准气体通入体积成正比。 The present invention adopts the following technical scheme: a direct quantitative verification method for the measurement of hydrolyzable fluoride in sulfur hexafluoride gas, which is characterized in that the easily hydrolyzed thionyl fluoride (SOF2) standard gas is selected as the quantitative basis, The SOF2 standard gas is passed into the absorption solution, the SOF2 standard gas is completely dissolved in the absorption solution, and the fluoride ion concentration in the absorption solution is directly proportional to the volume of the SOF2 standard gas.

优选地,吸收溶液为一定浓度的氢氧化钠溶液。 Preferably, the absorption solution is a certain concentration of sodium hydroxide solution.

优选地,SOF2标准气体的体积采用气体质量流量计进行计量。 Preferably, the volume of the SOF2 standard gas is measured by a gas mass flow meter.

优选地,吸收溶液中的氟离子浓度采用氟离子传感器进行测量。 Preferably, the fluoride ion concentration in the absorption solution is measured using a fluoride ion sensor.

优选地,具体包括如下步骤: Preferably, it specifically includes the following steps:

SS1气体吸收:以一定流速向氢氧化钠吸收溶液内通入SOF2标准气体,当气体质量流量计计量气体通入体积为n升时,停止进气,读取氟离子传感器测量数值,n为正数; SS1 gas absorption: Introduce SOF2 standard gas into the sodium hydroxide absorption solution at a certain flow rate, when the gas mass flowmeter measures the volume of gas introduced into n liters, stop the air intake, and read the measured value of the fluorine ion sensor, n is positive number;

SS2工作曲线绘制:重复步骤SS1操作,分别往吸收池内通入2n、3n、4n、5n、6n升气体,算出每次通入吸收池内氟离子的浓度,用氟离子传感器读取的数值与氟离子浓度绘制工作曲线; SS2 working curve drawing: repeat step SS1 operation, respectively pass 2n, 3n, 4n, 5n, 6n liters of gas into the absorption pool, calculate the concentration of fluorine ion in the absorption pool each time, use the value read by the fluorine ion sensor to compare with the fluorine ion Ion concentration drawing working curve;

SS3可水解氟化物含量测量:测量六氟化硫气体中可水解氟化物含量时,将氟离子传感器读取的数值在工作曲线上读出氟离子浓度,即可算出气体中可水解氟化物含量。 SS3 Measurement of hydrolyzable fluoride content: when measuring the content of hydrolyzable fluoride in sulfur hexafluoride gas, the value read by the fluoride ion sensor can be read from the working curve to read the fluoride ion concentration, and then the content of hydrolyzable fluoride in the gas can be calculated .

本发明所达到的有益效果:(1)本发明改变了以往配制标准溶液绘制工作曲线的方法,采用标准气体直接定量校验可水解氟化物的测量;(2)本发明解决了可水解氟化物测量试验工作量大、操作繁琐、平行试验误差大的难点,在保障试验准确性和稳定性的同时,提高了六氟化硫气体质量控制的效率,进一步保障充气电力设备的安全。 The beneficial effects achieved by the present invention: (1) The present invention changes the previous method of preparing a standard solution to draw a working curve, and uses standard gas to directly quantitatively verify the measurement of hydrolyzable fluoride; (2) The present invention solves the problem of hydrolyzable fluoride The difficulties of large measurement workload, cumbersome operation, and large parallel test error, while ensuring the accuracy and stability of the test, improve the efficiency of sulfur hexafluoride gas quality control and further ensure the safety of inflatable power equipment.

具体实施方式 Detailed ways

下面结合附图对本发明作进一步描述。以下实施例仅用于更加清楚地说明本发明的技术方案,而不能以此来限制本发明的保护范围。 The present invention will be further described below in conjunction with the accompanying drawings. The following examples are only used to illustrate the technical solution of the present invention more clearly, but not to limit the protection scope of the present invention.

本发明提出一种六氟化硫气体中可水解氟化物测量的直接定量校验方法,包括选取易水解的氟化亚硫酰(SOF2)标准气体作为定量的依据,将SOF2标准气体通入吸收溶液中,SOF2标准气体在吸收溶液中完全溶解,吸收溶液中的氟离子浓度与SOF2标准气体通入体积成正比。 The invention proposes a direct quantitative verification method for the measurement of hydrolyzable fluoride in sulfur hexafluoride gas, which includes selecting easily hydrolyzed thionyl fluoride (SOF2) standard gas as a quantitative basis, and passing the SOF2 standard gas into the absorption In the solution, the SOF2 standard gas is completely dissolved in the absorption solution, and the concentration of fluorine ions in the absorption solution is proportional to the volume of the SOF2 standard gas.

吸收溶液为一定浓度的氢氧化钠溶液;SOF2标准气体的体积采用气体质量流量计进行计量;吸收溶液中的氟离子浓度采用氟离子传感器进行测量;本发明具体包括如下步骤: The absorption solution is a sodium hydroxide solution of a certain concentration; SOF The volume of the standard gas is measured by a gas mass flowmeter; the fluoride ion concentration in the absorption solution is measured by a fluoride ion sensor; the present invention specifically includes the following steps:

SS1气体吸收:以一定流速向氢氧化钠吸收溶液内通入SOF2标准气体,当气体质量流量计计量气体通入体积为n升时,停止进气,读取氟离子传感器测量数值,n为正数; SS1 gas absorption: Introduce SOF2 standard gas into the sodium hydroxide absorption solution at a certain flow rate, when the gas mass flowmeter measures the volume of gas introduced into n liters, stop the air intake, and read the measured value of the fluorine ion sensor, n is positive number;

SS2工作曲线绘制:重复步骤SS1操作,分别往吸收池内通入2n、3n、4n、5n、6n升气体,算出每次通入吸收池内氟离子的浓度,用氟离子传感器读取的数值与氟离子浓度绘制工作曲线; SS2 working curve drawing: repeat step SS1 operation, respectively pass 2n, 3n, 4n, 5n, 6n liters of gas into the absorption pool, calculate the concentration of fluorine ion in the absorption pool each time, use the value read by the fluorine ion sensor to compare with the fluorine ion Ion concentration drawing working curve;

SS3可水解氟化物含量测量:测量六氟化硫气体中可水解氟化物含量时,将氟离子传感器读取的数值在工作曲线上读出氟离子浓度,即可算出气体中可水解氟化物含量。 SS3 Measurement of hydrolyzable fluoride content: when measuring the content of hydrolyzable fluoride in sulfur hexafluoride gas, the value read by the fluoride ion sensor can be read from the working curve to read the fluoride ion concentration, and then the content of hydrolyzable fluoride in the gas can be calculated .

本发明所达到的有益效果:(1)本发明改变了以往配制标准溶液绘制工作曲线的方法,采用标准气体直接定量校验可水解氟化物的测量;(2)本发明解决了可水解氟化物测量试验工作量大、操作繁琐、平行试验误差大的难点,在保障试验准确性和稳定想的同时,提高了六氟化硫气体质量控制的效率,进一步保障充气电力设备的安全。 The beneficial effects achieved by the present invention: (1) The present invention changes the previous method of preparing a standard solution to draw a working curve, and uses standard gas to directly quantitatively verify the measurement of hydrolyzable fluoride; (2) The present invention solves the problem of hydrolyzable fluoride The difficulties of large measurement workload, cumbersome operation, and large parallel test error, while ensuring the accuracy and stability of the test, improve the efficiency of sulfur hexafluoride gas quality control and further ensure the safety of inflatable power equipment.

以上所述仅是本发明的优选实施方式,应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明技术原理的前提下,还可以做出若干改进和变形,这些改进和变形也应视为本发明的保护范围。 The above is only a preferred embodiment of the present invention, it should be pointed out that for those of ordinary skill in the art, without departing from the technical principle of the present invention, some improvements and modifications can also be made. It should also be regarded as the protection scope of the present invention.

Claims (5)

1. the direct quantitative method of calibration of hydrolyzable fluoride measurement in a sulfur hexafluoride gas, it is characterized in that, that chooses facile hydrolysis fluoridizes thionyl (SOF2) calibrating gas as quantitative foundation, described SOF2 calibrating gas is passed in absorbent solution, described SOF2 calibrating gas dissolves completely in described absorbent solution, and the fluorinion concentration in described absorbent solution passes into volume to described SOF2 calibrating gas and is directly proportional.
2. the direct quantitative method of calibration of hydrolyzable fluoride measurement in a kind of sulfur hexafluoride gas according to claim 1, it is characterized in that, described absorbent solution is certain density sodium hydroxide solution.
3. the direct quantitative method of calibration of hydrolyzable fluoride measurement in a kind of sulfur hexafluoride gas according to claim 2, is characterized in that, the volume of described SOF2 calibrating gas adopts mass-flow gas meter to measure.
4. the direct quantitative method of calibration of hydrolyzable fluoride measurement in a kind of sulfur hexafluoride gas according to claim 3, is characterized in that, the fluorinion concentration in described absorbent solution adopts fluorine ion sensing device to measure.
5. the direct quantitative method of calibration of hydrolyzable fluoride measurement in a kind of sulfur hexafluoride gas according to claim 1, is characterized in that, specifically comprise the steps:
SS1 gas absorption: pass into SOF2 calibrating gas with certain flow rate in NaOH absorbent solution, when mass-flow gas meter meter gaseous pass into volume be n rise time, stop air inlet, read fluorine ion sensing device and measure numerical value, n is positive number;
SS2 working curve is drawn: repeating said steps SS1 operates, in absorption cell, pass into 2n, 3n, 4n, 5n, 6n respectively and rise gas, calculate the concentration at every turn passing into fluorine ion in absorption cell, the numerical value read with fluorine ion sensing device and fluorinion concentration drawing curve;
SS3 hydrolyzable content of fluoride is measured: when measuring hydrolyzable content of fluoride in sulfur hexafluoride gas, the numerical value that fluorine ion sensing device reads is read fluorinion concentration on working curve, can calculate hydrolyzable content of fluoride in gas.
CN201510189593.5A 2015-04-21 2015-04-21 A Direct Quantitative Calibration Method for the Measurement of Hydrolyzable Fluoride in Sulfur Hexafluoride Gas Active CN104807719B (en)

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Cited By (3)

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CN106324077A (en) * 2016-08-03 2017-01-11 西安交通大学 Gold-nanometer-hole-film ionizing thionyl-fluoride sensor
CN107525829A (en) * 2017-08-03 2017-12-29 国网安徽省电力公司电力科学研究院 The detection method of hydrolyzable content of fluoride in sulfur hexafluoride gas
CN107576708A (en) * 2017-08-03 2018-01-12 国网安徽省电力公司电力科学研究院 Hydrolyzable the Determination Method of Fluoride and device in sulfur hexafluoride gas

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106324077A (en) * 2016-08-03 2017-01-11 西安交通大学 Gold-nanometer-hole-film ionizing thionyl-fluoride sensor
CN106324077B (en) * 2016-08-03 2019-03-01 西安交通大学 A kind of Jenner's metre hole thin-film electro is fluorinated thionyl sensor from formula
CN107525829A (en) * 2017-08-03 2017-12-29 国网安徽省电力公司电力科学研究院 The detection method of hydrolyzable content of fluoride in sulfur hexafluoride gas
CN107576708A (en) * 2017-08-03 2018-01-12 国网安徽省电力公司电力科学研究院 Hydrolyzable the Determination Method of Fluoride and device in sulfur hexafluoride gas

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