CN111693481A - Determination of SF6Method for calibrating non-dispersive infrared absorption spectrum of CO content in gas - Google Patents
Determination of SF6Method for calibrating non-dispersive infrared absorption spectrum of CO content in gas Download PDFInfo
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- CN111693481A CN111693481A CN202010580154.8A CN202010580154A CN111693481A CN 111693481 A CN111693481 A CN 111693481A CN 202010580154 A CN202010580154 A CN 202010580154A CN 111693481 A CN111693481 A CN 111693481A
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- 238000000862 absorption spectrum Methods 0.000 title claims abstract description 19
- 238000010521 absorption reaction Methods 0.000 claims abstract description 62
- 238000000034 method Methods 0.000 claims abstract description 27
- 238000005259 measurement Methods 0.000 claims abstract description 24
- 230000003287 optical effect Effects 0.000 claims abstract description 13
- 238000001514 detection method Methods 0.000 claims abstract description 11
- 239000007789 gas Substances 0.000 claims description 101
- 238000001914 filtration Methods 0.000 claims description 6
- 238000012360 testing method Methods 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 238000003556 assay Methods 0.000 claims 8
- 229910018503 SF6 Inorganic materials 0.000 description 9
- 238000011088 calibration curve Methods 0.000 description 5
- SFZCNBIFKDRMGX-UHFFFAOYSA-N sulfur hexafluoride Chemical compound FS(F)(F)(F)(F)F SFZCNBIFKDRMGX-UHFFFAOYSA-N 0.000 description 5
- 238000004566 IR spectroscopy Methods 0.000 description 4
- 238000012545 processing Methods 0.000 description 3
- 230000005855 radiation Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 2
- 230000002238 attenuated effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000009421 internal insulation Methods 0.000 description 1
- 229960000909 sulfur hexafluoride Drugs 0.000 description 1
- OBTWBSRJZRCYQV-UHFFFAOYSA-N sulfuryl difluoride Chemical compound FS(F)(=O)=O OBTWBSRJZRCYQV-UHFFFAOYSA-N 0.000 description 1
- LSJNBGSOIVSBBR-UHFFFAOYSA-N thionyl fluoride Chemical compound FS(F)=O LSJNBGSOIVSBBR-UHFFFAOYSA-N 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
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3504—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing gases, e.g. multi-gas analysis
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3504—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing gases, e.g. multi-gas analysis
- G01N2021/3509—Correlation method, e.g. one beam alternating in correlator/sample field
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Abstract
The invention discloses a method for measuring SF6The calibration method of the non-dispersive infrared absorption spectrum of the CO content in the gas comprises the following steps: step 1, installing an optical filter for analyzing the absorption wavelength of gas in front of a detection end of a sensor; step 2, modulating the infrared light source by a GFC signal to obtain a reference light beam and a measuring light beam, and enabling the reference light beam and the measuring light beam to enter a third gas absorption cell in sequence; step 3, the reference beam and the measuring beam are absorbed by the standard gas in the third gas absorption cell in sequence and then received by the infrared detector through the optical filter; step 4, obtaining the difference voltage of the reference signal and the measurement signal through the reference signal and the measurement signal received by the infrared detector; step 5, completing CO infrared calibration through the concentration and the differential voltage of the standard gas; the sensor solves the technical problems that the sensor in the prior art is initially calibrated and inverted, and the practicability, the reliability and the like of use cannot be guaranteed.
Description
Technical Field
The invention belongs to the gas detection technology, and particularly relates to SF (sulfur hexafluoride) determination6A calibration method of non-dispersive infrared absorption spectrum of CO content in gas.
Background
SF for electric power industry6The equipment has wide application, and SF can be detected according to gas components6Latent faults inside the device, in particular those involving the internal insulation material, can be characterized by the CO content. However, since the infrared region SF6The fault-characteristic gas component present in the plant comprises SO2、H 20、CO2、SO2F2、SOF2、CF4Etc. for economical and accurate detection of SF in the infrared region where a large number of gas components are present6The content of CO in gas components is a difficult problem, and part of documents report that a tunable laser infrared absorption spectrometry is used for detecting SF6The laser for detecting the content of CO in the gas by the tunable laser infrared absorption spectrometry is expensive and has insufficient economy. The prior art patent 201920423930.6 mentions a detection system for detecting CO content by using a non-dispersive infrared absorption spectrometry, however, the patent does not mention an initial calibration and concentration inversion method for detecting CO content by using a non-dispersive infrared absorption spectrometry, and all sensors need to realize accurate detection, and the initial calibration and inversion must be completed before use to ensure the practicability and reliability of use; the prior art does not achieve this function.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: to provide a method for measuring SF6A calibration method of non-dispersive infrared absorption spectrum of CO content in gas aims to solve the technical problems that the sensor in the prior art is initially calibrated and inverted, and the practicability, reliability and the like of use cannot be guaranteed.
The technical scheme of the invention is as follows:
measurement of SF6The calibration method of the non-dispersive infrared absorption spectrum of the CO content in the gas comprises the following steps:
step 4, obtaining the difference voltage of the reference signal and the measurement signal through the reference signal and the measurement signal received by the infrared detector;
and 5, completing CO infrared calibration through the concentration of the standard gas and the difference voltage.
It still includes: and 6, performing concentration inversion through the calibration result, and introducing gas with a certain standard concentration to test the calibrated sensor.
The method for enabling the reference light beam and the measuring light beam obtained after GFC signal modulation to enter the gas absorption cell sequentially comprises the following steps:
step 2.1, arranging an infrared light source at one side of the rotating filtering related wheel;
step 2.2, embedding a first gas absorption cell and a second gas absorption cell which can penetrate through an infrared light source on the rotating filtering related wheel; the first gas absorption cell is filled with high-concentration gas and is called a reference cell; the second gas absorption cell is filled with nitrogen and is called a measurement cell;
step 2.3, when the infrared light source passes through the reference cell, all infrared light at the characteristic absorption peak of the high-concentration gas is absorbed by the standard gas, and the light energy entering the first gas absorption cell is set as I0X, X represents a high concentration gas; the beam is a reference beam; the light energy of infrared light passing through the measuring cell at the characteristic absorption peak of the gas has no change, and the light energy is set as I0N2The light beam is a measuring light beam;
and 2.4, the reference light beam and the measuring light beam sequentially enter a third gas absorption cell.
Step 4, the method for obtaining the difference voltage of the reference signal and the measurement signal through the reference signal and the measurement signal received by the infrared detector comprises the following steps: converting the reference signal and the measurement signal into voltage signals by an infrared detector, and establishing a linear relation ln (V) between the absorption intensity and the concentration of the reference signal and the measurement signalO/V1) C, modeling based on the linear relationship, V0A voltage signal that is a measurement signal; v1Being reference signalsA voltage signal.
The CO infrared calibration method in the step 5 comprises the following steps:
the CO concentration signal is related to the voltage difference Δ U, where Δ U ═ V0-V1；V0Is the voltage of the measurement signal; v1Is the voltage of the reference signal; firstly, introducing CO standard gas with different concentrations, and measuring corresponding delta U, which is shown in the following table
| Voltage difference Δ U (mV) | SF6 standard concentration value of CO (μ L/L) for bottom gas |
| 1.33 | 0 |
| 48.1 | 10 |
| 71.6 | 15 |
| 95.1 | 20 |
| 140 | 30 |
| 234 | 50 |
| 470 | 100 |
| 703 | 150 |
| 937 | 200 |
| 1408 | 300 |
| 1874 | 400 |
| 2345 | 500 |
| 2809 | 600 |
| 3745 | 800 |
| 4681 | 1000 |
As can be seen from the above table, the linear relationship between the voltage signal and the concentration signal of the infrared absorption of CO is:
y＝0.2136x-0.2845
calculating the concentration by using the linear formula, and establishing a calibration linear curve; x is the voltage difference Δ U, and y is the CO gas concentration.
The method for performing concentration inversion through the calibration result in the step 6 comprises the following steps: gas with certain standard concentration is introduced to test the calibrated sensor, and the specific test result is shown in the following table:
The characteristic absorption peak refers to the absorption spectrum of CO of 4.65 μm and the absorption coefficient of 2150.58cm-1To (3).
The high concentration gas is SF6 to CO at a volume ratio of 1 to 1.
The invention has the beneficial effects that:
the invention realizes the infrared light signal modulation by a GFC (gas filter correction) turntable, divides measuring beams and reference beams by the GFC turntable, respectively inputs the measuring beams and the reference beams into a third gas absorption cell, then a narrow-band filter is arranged in front of the detection sensor, so that the signal change of the sensor only reflects the change of the concentration of the gas to be detected, the detection accuracy is improved, finally, the relation between the absorption intensity and the concentration is obtained through data processing, a calibration curve is established to realize the calibration of the sensor, finally, the concentration inversion of the sensor can be realized through the calibration curve, the sensor is tested, the problems that the prior art does not have initial calibration and concentration inversion for detecting the CO content by a non-dispersive infrared absorption spectrum method, all sensors can realize accurate detection, before use, initial calibration and inversion must be completed to ensure the practicability and reliability of use.
Drawings
FIG. 1 is a schematic view of the detecting device of the present invention;
FIG. 2 is a schematic diagram of a CO calibration curve according to the present invention.
Detailed Description
The realization principle of the invention is as follows: the degree of absorption of the different wavelengths of infrared radiation by the various substances is not uniform, and thus when the different wavelengths of infrared radiation are sequentially irradiated onto the sample substance, a characteristic absorption is formed as certain wavelengths of radiation are selectively absorbed by the sample and attenuated. The absorption relationship obeys Lambert-Beer absorption law. The incident light is parallel light, and the same incident light can be directly measured to obtain a constant value with intensity I0The intensity of emergent light is I, and the measuring optical path length of the gas medium is L.
When the intensity of the light decreases to dI due to the absorption of the number of molecules dN in the gaseous medium, according to the lambert-beer law:
dI/I＝-KdN
wherein K is a proportionality constant and is obtained by integration:
lnI＝-KN+α
wherein N is the total number of molecules of the gas-absorbing medium, and α is an integral constant, i.e., lnI0(ii) a Obviously, N ^ CL, C is the gas concentration, the formula can be written as:
I＝exp(α)exp(-KN)
I＝exp(α)exp(-μCL)
I＝I0exp(-μCL)
wherein C is the concentration of the gas to be measured, L is the length of the measuring optical path, namely the length of the gas chamber, mu is the absorption coefficient of the gas molecules.
As can be seen from the formula, the light intensity decays exponentially in the gas medium along with the concentration C and the length L; the absorption coefficient depends on the gas properties, and the absorption coefficients μ of the various gases differ from each other, μ being a constant for a particular gas, and L being the length of the gas cell, also a determined constant.
Therefore, the invention selects the absorption spectrum of CO to be 4.65 μm and the absorption coefficient to be 2150.58cm-1As the characteristic absorption peak of CO gas.
Because multiple mixed gas components exist in the SF6 device, in order to analyze specific components, a narrow-band filter suitable for analyzing the absorption wavelength of gas is arranged in front of a sensor or an infrared light source, so that the signal change of the sensor only reflects the concentration change of the gas to be detected, the detection precision is improved, and the interference by other impurities is avoided.
The invention is realized by a GFC turntable, a gas absorption pool and a signal receiving and processing part; infrared light emitted by the infrared LED light source 2 enters the third gas absorption cell 5 after being modulated by a GFC signal, is fully absorbed by gas in the third gas absorption cell, passes through the optical filter 6, is received by the infrared detector 7, and finally is subjected to data processing to obtain a voltage signal of the actually measured gas.
As shown in figure 1, the main working process of the GFC wheel disc is to modulate incident continuous infrared light through a filtering related wheel, a first gas absorption cell 3 and a second gas absorption cell 4 which can transmit infrared incident light are arranged on the filtering related wheel, and the first gas absorption cell 3 is filled with high-concentration gasGas of high concentration of SF in gas6And CO in a volume ratio of 1 to 1; this cell is called the reference cell; the second gas absorption cell 4 is filled with N2Referred to as a measurement cell. When infrared incident light passes through the reference cell, almost all infrared light at the characteristic absorption peak of the gas is absorbed by the high-concentration gas, and the light energy entering the first absorption cell at the position is set as I0X (X represents a gas), and the infrared light passing through the measuring cell has almost no change in the light energy at the characteristic absorption peak of the gas, which is designated as I0N2. The GFC wheel disc rotates at a constant speed under the driving of the motor 1, and the two modulated beams of light successively and repeatedly enter the third gas absorption cell and are measured through the infrared detector 7.
Converting the measured reference signal and the measured signal into voltage signals through a sensor; obtaining a linear relation ln (V) between absorption intensity and concentration through a voltage signalO/V1) C, establishing a model based on the linear relation.
CO infrared calibration process
As can be seen from the above, the CO concentration signal is related to the difference voltage Δ U, where Δ U ═ V0-V1；VOIs a measurement signal; v1Is a reference signal; firstly, SF with different concentrations is introduced into a third gas absorption tank6For the CO gas of the bottom gas, the corresponding Δ U was measured, as shown in the following table
As can be seen from the above table, the voltage signal of CO infrared absorption has a good linear relationship with the concentration signal, wherein the linear relationship is as follows:
y＝0.2136x-0.2845
and (5) performing concentration calculation by using the linear formula to establish a calibration curve. x is the voltage difference Δ U, and y is the CO gas concentration.
Performing concentration inversion on the established calibration curve, namely introducing CO gas with SF6 of certain standard concentration as bottom gas to test the calibrated sensor, see the following table
As can be seen from the above table: when the measured value is less than or equal to 50 mu L/L, the error is less than or equal to +/-3 mu L/L; when the measured value is more than 50 mu L/L, the relative error is less than or equal to +/-6 percent.
Claims (9)
1. Measurement of SF6The calibration method of the non-dispersive infrared absorption spectrum of the CO content in the gas comprises the following steps:
step 1, installing an optical filter for analyzing the absorption wavelength of gas in front of a detection end of a sensor;
step 2, modulating the infrared light source by a GFC signal to obtain a reference light beam and a measuring light beam, and enabling the reference light beam and the measuring light beam to enter a third gas absorption cell in sequence;
step 3, the reference beam and the measuring beam are absorbed by the standard gas in the third gas absorption cell in sequence and then received by the infrared detector through the optical filter;
step 4, obtaining the difference voltage of the reference signal and the measurement signal through the reference signal and the measurement signal received by the infrared detector;
and 5, completing CO infrared calibration through the concentration of the standard gas and the difference voltage.
2. An assay SF according to claim 16The calibration method of the non-dispersive infrared absorption spectrum of the CO content in the gas is characterized by comprising the following steps: it still includes: and 6, performing concentration inversion through the calibration result, and introducing CO gas with a certain standard concentration to test the calibrated sensor.
3. An assay SF according to claim 16In gasThe calibration method of the non-dispersive infrared absorption spectrum of the CO content is characterized by comprising the following steps: the method for enabling the reference light beam and the measuring light beam obtained after GFC signal modulation to enter the gas absorption cell sequentially comprises the following steps:
step 2.1, arranging an infrared light source at one side of the rotating filtering related wheel;
step 2.2, embedding a first gas absorption cell and a second gas absorption cell which can penetrate through an infrared light source on the rotating filtering related wheel; the first gas absorption cell is filled with high-concentration gas and is called a reference cell; the second gas absorption cell is filled with nitrogen and is called a measurement cell;
step 2.3, when the infrared light source passes through the reference cell, all infrared light at the characteristic absorption peak of the high-concentration gas is absorbed by the standard gas, and the light energy entering the first gas absorption cell is set as I0X, X represents a high concentration gas; the beam is a reference beam; the light energy of infrared light passing through the measuring cell at the characteristic absorption peak of the gas has no change, and the light energy is set as I0N2The light beam is a measuring light beam;
and 2.4, enabling the reference light beam and the measuring light beam to enter a third gas absorption cell in sequence.
4. An assay SF according to claim 16The calibration method of the non-dispersive infrared absorption spectrum of the CO content in the gas is characterized by comprising the following steps: step 4, the method for obtaining the difference voltage of the reference signal and the measurement signal through the reference signal and the measurement signal received by the infrared detector comprises the following steps: converting the reference signal and the measurement signal into voltage signals by an infrared detector, and establishing a linear relation ln (V) between the absorption intensity and the concentration of the reference signal and the measurement signalO/V1) C, modeling based on the linear relationship, V0A voltage signal that is a measurement signal; v1Is a voltage signal of the reference signal.
5. An assay SF according to claim 16The calibration method of the non-dispersive infrared absorption spectrum of the CO content in the gas is characterized by comprising the following steps: the CO infrared calibration method in the step 5 comprises the following steps:
the CO concentration signal is related to a difference voltage Δ U, where Δ U ═ V0-V1；V0A voltage signal that is a measurement signal; v1A voltage signal that is a reference signal; firstly, introducing CO standard gas with different concentrations, and measuring corresponding delta U, which is shown in the following table
As can be seen from the above table, the linear relationship between the voltage signal and the concentration signal of the infrared absorption of CO is:
y＝0.2136x-0.2845
calculating the concentration by using the linear formula, and establishing a calibration linear curve; x is the voltage difference Δ U, and y is the CO gas concentration.
6. An assay SF according to claim 26The calibration method of the non-dispersive infrared absorption spectrum of the CO content in the gas is characterized by comprising the following steps: the method for performing concentration inversion through the calibration result in the step 6 comprises the following steps: the calibrated sensor is tested by introducing CO gas with a certain standard concentration, and the specific test result is shown in the following table:
7. an assay SF according to claim 16The calibration method of the non-dispersive infrared absorption spectrum of the CO content in the gas is characterized by comprising the following steps: step 1, the optical filter is a narrow-band optical filter.
8. According to claimAn assay as claimed in claim 36The calibration method of the non-dispersive infrared absorption spectrum of the CO content in the gas is characterized by comprising the following steps: the characteristic absorption peak refers to the absorption spectrum of CO of 4.65 μm and the absorption coefficient of 2150.58cm-1To (3).
9. An assay SF according to claim 36The calibration method of the non-dispersive infrared absorption spectrum of the CO content in the gas is characterized by comprising the following steps: the high concentration gas is SF6The volume ratio to CO is 1 to 1.
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| CN112595687A (en) * | 2020-11-24 | 2021-04-02 | 南京工业大学 | Non-dispersive infrared gas concentration detection device and method with same optical axis |
| CN112697747A (en) * | 2020-12-04 | 2021-04-23 | 贵州电网有限责任公司 | Device and method for detecting decomposer, moisture and purity in sulfur hexafluoride gas |
| CN114002176A (en) * | 2021-12-06 | 2022-02-01 | 国网江苏省电力有限公司检修分公司 | SF6 decomposition component gas detection device based on ultraviolet absorption spectrum |
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