CN117347431A - Perfluorinated hexanone gas concentration detection system and detection method based on thermal conductivity principle - Google Patents
Perfluorinated hexanone gas concentration detection system and detection method based on thermal conductivity principle Download PDFInfo
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- CN117347431A CN117347431A CN202311314923.XA CN202311314923A CN117347431A CN 117347431 A CN117347431 A CN 117347431A CN 202311314923 A CN202311314923 A CN 202311314923A CN 117347431 A CN117347431 A CN 117347431A
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- 238000001514 detection method Methods 0.000 title claims abstract description 170
- QQZOPKMRPOGIEB-UHFFFAOYSA-N 2-Oxohexane Chemical class CCCCC(C)=O QQZOPKMRPOGIEB-UHFFFAOYSA-N 0.000 title claims abstract description 127
- 239000007789 gas Substances 0.000 claims abstract description 214
- WVSNNWIIMPNRDB-UHFFFAOYSA-N 1,1,1,3,3,4,4,5,5,6,6,6-dodecafluorohexan-2-one Chemical compound FC(F)(F)C(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F WVSNNWIIMPNRDB-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000012159 carrier gas Substances 0.000 claims abstract description 44
- 238000002360 preparation method Methods 0.000 claims abstract description 41
- 238000000034 method Methods 0.000 claims abstract description 25
- 230000001105 regulatory effect Effects 0.000 claims description 67
- 238000011088 calibration curve Methods 0.000 claims description 24
- 238000005259 measurement Methods 0.000 claims description 9
- 230000008859 change Effects 0.000 claims description 8
- 238000012360 testing method Methods 0.000 claims description 8
- 238000007599 discharging Methods 0.000 claims description 6
- 238000012545 processing Methods 0.000 claims description 6
- 238000004458 analytical method Methods 0.000 abstract description 3
- 230000035945 sensitivity Effects 0.000 abstract description 2
- 238000012423 maintenance Methods 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 230000008901 benefit Effects 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- PXBRQCKWGAHEHS-UHFFFAOYSA-N dichlorodifluoromethane Chemical compound FC(F)(Cl)Cl PXBRQCKWGAHEHS-UHFFFAOYSA-N 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 229920004449 Halon® Polymers 0.000 description 1
- 238000004566 IR spectroscopy Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000012983 electrochemical energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000004817 gas chromatography Methods 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
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000009965 odorless effect Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 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
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/20—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity
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Abstract
The application provides a perfluoro-hexanone gas concentration detecting system and a detecting method based on a thermal conductivity principle, which belong to the technical field of fire protection detection and comprise the following steps: the device comprises a gas mixing preparation device, a container to be tested and a detection device; firstly, inputting perfluorinated hexanone gases with different concentrations into a detection device through a gas mixing preparation device to serve as calibration comparison data; when the perfluorohexanone gas sample is required to be detected on site, the perfluorohexanone gas sample in the container to be detected is introduced into the detection device through the second air inlet, and the thermal conductivity of the mixed gas of the perfluorohexanone standard gas and the carrier gas is compared and calibrated, so that the thermal conductivity of the sensitive element in the perfluorohexanone gas sample is obtained, the concentration of the perfluorohexanone gas sample is detected, the method has the characteristics of simplicity, rapidness, low analysis cost and high sensitivity, the on-site rapid detection of the perfluorohexanone gas is realized, the method is convenient for production line operation and maintenance personnel to use, and the method has important significance in reducing the supervision cost and improving the supervision efficiency.
Description
Technical Field
The application belongs to the technical field of fire protection detection, and particularly relates to a perfluorinated hexanone gas concentration detection system and method based on a thermal conductivity principle.
Background
The perfluoro-hexanone is colorless, odorless and transparent liquid at normal temperature, is easy to vaporize, and has a molecular formula of C 6 F 12 O is an important halon extinguishing agent substitute, has the advantages of low extinguishing concentration, high cooling speed, high safety coefficient, strong insulativity, cleanness, environmental protection and the like, can extinguish A, B, C, E, F fire and electric fire, and is widely applied to places such as electrochemical energy storage power stations, oil immersed transformers, high-low voltage distribution rooms, information machine rooms, data centers and the like.
At present, the detection of the concentration of the perfluorinated hexanone is mainly finished by a gas chromatography method, a differential pressure method and an infrared absorption spectrometry method, and the methods are used for laboratory analysis and detection due to higher sensitivity and selectivity, but the methods have the advantages of complex detection process, long time consumption and high detection cost, and the detection needs to be finished by a professional instrument through operation of a professional, so that the requirements of the on-site rapid analysis and detection of the concentration of the perfluorinated hexanone are difficult to meet.
Disclosure of Invention
The present application aims to solve at least one of the technical problems existing in the prior art or related technologies.
To this end, the application provides a perfluoro hexanone gas concentration detecting system based on thermal conductivity principle, includes: the device comprises a gas mixing preparation device, a container to be tested and a detection device; the gas mixing preparation device comprises a first inlet, a second inlet and an outlet, wherein the first inlet is used for introducing the standard gas of the perfluorinated hexanone, the second inlet is used for introducing the carrier gas, and the gas mixing preparation device is used for mixing the standard gas of the perfluorinated hexanone with the carrier gas; a perfluorinated hexanone gas sample is arranged in the container to be tested; the detection device comprises a first air inlet, a second air inlet and an air outlet, wherein the first air inlet is detachably connected with the air outlet, the second air inlet is detachably connected with the container to be detected, a sensitive element is arranged in the detection device, and the detection device is used for measuring the concentration of gas according to the change of the heat conductivity coefficient of the sensitive element under the constant temperature condition.
In addition, the perfluorinated hexanone gas concentration detection system based on the thermal conductivity principle in the technical scheme provided by the application can also have the following additional technical characteristics:
in a possible embodiment, the perfluorinated hexanone gas concentration detection system based on the thermal conductivity principle further comprises: the device comprises a first regulating valve, a second regulating valve and a deflation port; the first regulating valve is arranged on the first inlet and is used for regulating the flow of the standard gas of the perfluorinated hexanone; the second regulating valve is arranged on the second inlet and is used for regulating the flow of the carrier gas so as to regulate the mixing proportion of the standard gas of the perfluorinated hexanone and the carrier gas; the air discharging opening is arranged on the mixed air preparation device and is used for discharging residual air in the mixed air preparation device.
In a possible embodiment, the perfluorinated hexanone gas concentration detection system based on the thermal conductivity principle further comprises: a third regulating valve and a fourth regulating valve; the third regulating valve is arranged on the first air inlet and is used for regulating the flow of the gas entering the detection device from the gas mixing preparation device; the fourth regulating valve is arranged on the second air inlet and is used for regulating the flow of the perfluorinated hexanone gas sample entering the detection device.
In one possible implementation mode, the detection device detects the concentration of the perfluorinated hexanone gas sample in the container to be detected according to the change of the heat conductivity coefficient of the sensing element in the mixed gas of the perfluorinated hexanone standard gas and the carrier gas.
In a possible embodiment, the detection device further comprises: the device comprises a detection pool, an acquisition module, a processing module and a display module; the detection cell is used for containing gas, and the sensitive element is used for adsorbing the gas in the detection cell; the acquisition module is used for acquiring the heat conductivity coefficient variation of the sensitive element under the constant temperature condition; the processing module is used for converting the acquired heat conductivity coefficient variable quantity into a voltage variable quantity; the display module is used for displaying the measurement result.
In another aspect of the present application, a method for detecting a concentration of a perfluorohexanone gas based on a thermal conductivity principle is provided, and the method for detecting a concentration of a perfluorohexanone gas based on a thermal conductivity principle includes: preheating a detection system, determining a background value, drawing a calibration curve and testing sample concentration; electrifying and preheating a detection system to keep the temperature of a detection device stable; introducing carrier gas into the mixed gas preparation device, and enabling the carrier gas to flow through the detection device to obtain a first detection value which is used as a background value of the detection system; and (3) introducing the standard gas and the carrier gas of the perfluorinated hexanone into the mixed gas preparation device, enabling the mixed gas with different proportions to flow through the detection device, respectively obtaining second detection values, drawing a calibration curve of the concentration of the perfluorinated hexanone, introducing the perfluorinated hexanone gas sample into the detection device, obtaining a third detection value, calibrating the third detection value according to the calibration curve, and calculating the concentration of the perfluorinated hexanone sample.
In a possible embodiment, determining the background value further comprises: adjusting the third adjusting valve to enable the carrier gas to flow through the detection device at a flow rate of not more than 200 mL/min; repeating the measurement for at least 3 times, obtaining at least 3 first detection values, and taking the arithmetic average value of the first detection values as a background value.
In one possible embodiment, the drawing of the calibration curve further comprises: the first regulating valve and the second regulating valve are regulated to ensure that the output concentration of the gas mixing preparation device is respectively 0%, 50%, 80%, 85%, 90%, 95% and 100% of the mixed gas of the standard gas of the perfluorinated hexanone and the carrier gas; adjusting the third adjusting valve to enable the mixed gas to flow through the detection device at a flow rate of not more than 200 mL/min; and repeatedly measuring the mixed gas of each concentration at least 3 times, respectively obtaining at least 3 second detection values of the mixed gas of each concentration, respectively taking an arithmetic average value, and drawing a calibration curve.
In one possible embodiment, the test sample concentration further comprises: adjusting a fourth adjusting valve to enable the perfluorinated hexanone gas sample to flow through the detection device at a flow rate of not more than 200 mL/min; repeatedly measuring the perfluorinated hexanone gas sample for at least 3 times, obtaining at least 3 third detection values, taking the arithmetic average value of the third detection values as an indication value of the detection device, and then calculating the concentration of the perfluorinated hexanone sample according to a calibration curve.
In a possible embodiment, after calculating the concentration of the perfluorinated hexanone sample, further comprising: when the concentration of the perfluorinated hexanone sample is more than or equal to 90%, judging that the perfluorinated hexanone gas sample meets the requirements; and when the concentration of the perfluorinated hexanone sample is less than 90%, judging that the concentration of the perfluorinated hexanone does not meet the requirement.
The utility model provides a perfluoro hexanone gas concentration detecting system and method based on thermal conductance principle, compares with prior art, and beneficial effect is:
the invention quantitatively analyzes the perfluorohexanone gas sample based on the difference of the thermal conductivity coefficients of the sensitive element in the gas to be detected and the background gas, and obtains the thermal conductivity coefficient of the sensitive element in the perfluorohexanone gas sample by comparing and calibrating the thermal conductivity coefficients of the mixed gas of the perfluorohexanone standard gas and the carrier gas, thereby detecting the concentration of the perfluorohexanone gas sample.
Drawings
Various other advantages and benefits will become apparent to those of ordinary skill in the art upon reading the following detailed description of the preferred embodiments. The drawings are only for purposes of illustrating the preferred embodiments and are not to be construed as limiting the application. Also, like reference numerals are used to designate like parts throughout the figures. In the drawings:
fig. 1 is a schematic structural diagram of a system for detecting the concentration of a perfluorinated hexanone gas based on the thermal conductivity principle according to an embodiment of the present application;
fig. 2 is a schematic structural diagram of a detection device in a perfluoro-hexanone gas concentration detection system based on the thermal conductivity principle according to an embodiment of the present application;
FIG. 3 is a schematic diagram of a system for detecting the concentration of a perfluorinated hexanone gas based on the thermal conductivity principle according to one embodiment of the present application;
fig. 4 is a flow chart of a method for detecting concentration of perfluorohexanone gas according to an embodiment of the present disclosure;
fig. 5 is a flow chart of a method for detecting concentration of perfluorohexanone gas according to another embodiment of the present disclosure;
wherein, the correspondence between the reference numerals and the component names in fig. 1 to 5 is:
10. a gas mixing preparation device; 11. a container to be measured; 12. a detection device; 121. a sensor; 122. an acquisition module; 123. a processing module; 124. a display module; 125. a detection pool; 13. a first regulating valve; 14. a second regulating valve; 15. a vent port; 16. a third regulating valve; 17. and a fourth regulating valve.
Detailed Description
In the description of the present application, it is to be understood that, the terms "center", "longitudinal", "transverse", and "longitudinal" length, width, and thickness, upper, lower, front, rear, left, right, and the like,
The references to orientation or positional relationships "vertical," "horizontal," "top," "bottom," "inner," "outer," "clockwise," "counterclockwise," etc., are based on the orientation or positional relationships shown in the drawings, are merely for convenience of description and to simplify the description, and do not indicate or imply that the devices or elements referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore should not be construed as limiting the present application.
Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more such feature. In the description of the present application, the meaning of "a plurality" is two or more, unless explicitly defined otherwise.
In the present application, unless explicitly specified and limited otherwise, the terms "mounted," "connected," "secured," and the like are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium, and can be communication between two elements. The specific meaning of the terms in this application will be understood by those of ordinary skill in the art as the case may be.
The preferred embodiments of the present application will be described below with reference to the accompanying drawings, it being understood that the preferred embodiments described herein are for illustration and explanation of the present application only and are not intended to limit the present application.
Referring now to fig. 1 to 3 in combination, according to an embodiment of the present application, a system for detecting the concentration of a perfluorohexanone gas based on the thermal conductivity principle comprises: a gas mixing preparation device 10, a container 11 to be tested and a detection device 12; the gas mixing preparation device 10 comprises a first inlet, a second inlet and an outlet, wherein the first inlet is used for introducing the standard gas of the perfluorinated hexanone, the second inlet is used for introducing the carrier gas, and the gas mixing preparation device 10 is used for mixing the standard gas of the perfluorinated hexanone with the carrier gas; the container 11 to be measured is internally provided with a perfluorinated hexanone gas sample; the detection device 12 comprises a first air inlet, a second air inlet and an air outlet, wherein the first air inlet is detachably connected with the air outlet, the second air inlet is detachably connected with the container 11 to be detected, a sensing element 121 is arranged in the detection device 12, and the detection device 12 is used for measuring the concentration of gas according to the change of the thermal conductivity coefficient of the sensing element 121 under the constant temperature condition.
The system for detecting the concentration of the perfluorinated hexanone gas based on the thermal conductivity principle comprises a detection device 12 detachably connected with a gas mixing preparation device 10 and a container 11 to be detected, wherein before a perfluorinated hexanone gas sample is detected on site, perfluorinated hexanone standard gas and carrier gas are respectively introduced into the gas mixing preparation device 10 through a first inlet and a second inlet, so that the mixing proportion of the perfluorinated hexanone standard gas and the carrier gas is quickly adjusted, and the perfluorinated hexanone gas with different concentrations is input into the detection device 12 from an outlet to serve as calibration comparison data; when the perfluorohexanone gas sample needs to be detected on site, the gas mixing preparation device 10 is dismantled, the perfluorohexanone gas sample in the container 11 to be detected is introduced into the detection device 12 through the second air inlet, and the thermal conductivity coefficient of the sensing element 121 can be changed when different gases are adsorbed, so that the detection value of the perfluorohexanone gas sample is compared and calibrated according to the test value of the perfluorohexanone gas with different concentrations, the accuracy and the effectiveness of the detection of the perfluorohexanone gas sample are improved, and the on-site rapid detection of the perfluorohexanone sample is realized.
Further, since the temperature of the sensing element 121 is constant, the temperature of the sensing element 121 can be set as a temperature standard parameter, and the temperature compensation is performed on the environment where the sensing element 121 is located, so as to ensure that the sensing element 121 is under a constant temperature condition, thereby improving the detection performance of the detection system and reducing the measurement error caused by the change of the environmental temperature.
Preferably, the detection system and the connecting pipeline are made of corrosion-resistant stainless steel materials because the perfluorinated hexanone has weak corrosiveness, so that the detection performance of the detection system is maintained.
As shown in fig. 1, in one possible embodiment, a first regulating valve 13 is provided on the first inlet port, the first regulating valve 13 being used to regulate the flow of the standard gas of perfluoro hexanone; the second regulating valve 14 is arranged on the second inlet, and the second regulating valve 14 is used for regulating the flow of the carrier gas so as to regulate the mixing proportion of the standard gas of the perfluorinated hexanone and the carrier gas; the air release opening 15 is provided in the air-mixing preparation device 10, and the air release opening 15 is used for discharging the residual air in the air-mixing preparation device 10.
In the technical scheme, a first regulating valve 13 is arranged on a first inlet to quickly regulate the flow of the standard gas of the perfluorinated hexanone into the gas mixing preparation device 10; the second regulating valve 14 is arranged on the second inlet to quickly regulate the flow of the carrier gas entering the gas mixing preparation device 10, so that the mixing proportion of the standard perfluorinated hexanone gas and the carrier gas in the gas mixing preparation device 10 is quickly regulated to obtain perfluorinated hexanone gases with different concentrations; through setting up the relief vent 15 on mixing gas preparation device 10 to be convenient for with mixing gas preparation device 10 in the residual gas exhaust clean, avoid mixing gas preparation device 10 in the residual gas influence perfluorohexanone gas concentration, prevent predetermined perfluorohexanone gas concentration change, in order to ensure when adjusting first governing valve 13 and second governing valve 14, can carry out accurate regulation to the concentration of perfluorohexanone gas, guarantee the accuracy nature of comparison calibration data, thereby ensure the accuracy nature to the final measuring result of perfluorohexanone gas sample.
It should be noted that, the air release port 15 is provided with a sealing cover, when the standard gas of perfluoro-hexanone and the carrier gas are introduced into the gas mixing and preparing device 10, the sealing cover is kept in an opened state, and the first regulating valve 13 and the second regulating valve 14 are regulated until the concentration of the perfluoro-hexanone gas in the gas mixing and preparing device 10 reaches a preset value, and then the sealing cover is covered, so that the mixed gas in the gas mixing and preparing device 10 is introduced into the detecting device 12 in a constant concentration, and the accuracy of the detection result is ensured.
As shown in fig. 1, in one possible embodiment, a third regulating valve 16 is provided on the first air inlet, the third regulating valve 16 being used to regulate the flow rate of the gas from the gas-mixing and preparing device 10 into the detecting device 12; a fourth regulating valve 17 is arranged on the second inlet, the fourth regulating valve 17 being used for regulating the flow rate of the sample of perfluorohexanone gas into the detection device 12.
In the technical scheme, the third regulating valve 16 is arranged on the first air inlet to regulate the flow rate of the gas output by the gas mixing preparation device 10, so that the mixed perfluorinated hexanone gas flows through the detection device 12 at a moderate flow rate, the problems of short detection response time and inaccurate detection result of the detection device 12 caused by overlarge flow rate are avoided, meanwhile, the problems of slower acquisition speed of comparison calibration data caused by overlarge flow rate are avoided, and the detection device 12 has enough accuracy while the detection efficiency is ensured; the fourth regulating valve 17 is arranged on the second air inlet to regulate the flow rate of the perfluorinated hexanone gas sample entering the detection device 12, so that the perfluorinated hexanone gas sample flows through the detection device 12 at a moderate flow rate, the detection accuracy of the perfluorinated hexanone gas sample by the detection device 12 and the detection efficiency on site are ensured, and the rapid detection of the perfluorinated hexanone gas sample on site is ensured.
In a possible embodiment, the detection device 12 detects the concentration of the perfluorohexanone gas sample in the container 11 to be detected according to the thermal conductivity coefficient variation of the sensing element 121 in the mixed gas of the perfluorohexanone standard gas and the carrier gas.
In the technical scheme, the detection device 12 quantitatively analyzes the perfluorinated hexanone gas sample according to the difference of heat conductivity coefficients of the sensing element 121 after adsorbing different gases; under the condition of the same temperature, the higher the concentration of the perfluorinated hexanone, the lower the heat conductivity coefficient of the sensitive element 121, the difference is obvious, and the heat conductivity coefficient of the sensitive element 121 in the perfluorinated hexanone gas sample can be obtained by comparing and calibrating the heat conductivity coefficients of the mixed gas of the perfluorinated hexanone standard gas and the carrier gas, so that the concentration of the perfluorinated hexanone gas sample can be simply, quickly and accurately obtained.
As shown in fig. 2, in one possible embodiment, the detection cell 125 is configured to contain a gas, and the sensing element 121 is configured to adsorb the gas within the detection cell 125; the collection module 122 is used for collecting the thermal conductivity coefficient variation of the sensitive element 121 under the constant temperature condition; the processing module 123 is configured to convert the collected thermal conductivity variable into a voltage variable; the display module 124 is used for displaying the measurement result.
In this technical scheme, the detection tank 125 is communicated with the gas mixing preparation device 10 and the container 11 to be detected, and the thermal conductivity coefficient of the sensing element 121 after adsorbing the gas in the detection tank 125 changes according to the concentration of the gas; the change amount of the thermal conductivity coefficient of the sensing element 121 after absorbing gas at constant temperature is collected by the collecting module 122, calculated by the processing module 123 and converted into the voltage change amount, and the final measurement result is displayed by the display module 124, so that the concentration or content of the perfluorinated hexanone gas sample can be intuitively read on site.
The higher the concentration of the perfluorinated hexanone is, the smaller the heat conductivity coefficient of the sensitive element is, and the linear relation is formed.As shown in fig. 3, the linear relationship can be expressed as:wherein x represents the relative concentration of the perfluorohexanone gas sample to be detected, K x Represents the heat conductivity coefficient, K of the sensitive element measured in the perfluorohexanone gas sample to be measured 0 The heat conductivity coefficient, K of the sensitive element when the concentration of the perfluorinated hexanone gas is 0 percent 100 The heat conductivity coefficient of the sensing element when the concentration of the perfluorinated hexanone gas is 100 percent is shown. Therefore, the relative concentration of the current perfluorinated hexanone gas sample can be rapidly obtained by measuring the heat conductivity coefficient of the sensitive element in the perfluorinated hexanone gas sample with the concentration of 100%, the concentration of 0% and the perfluorinated hexanone gas sample to be measured.
According to a second aspect of the present application, referring to fig. 4 in combination, a method for detecting the concentration of a perfluorinated hexanone gas based on the thermal conductivity principle is provided, and the system for detecting the concentration of a perfluorinated hexanone gas based on the thermal conductivity principle according to any one of the above technical solutions is adopted, and includes: preheating a detection system, determining a background value, drawing a calibration curve and testing sample concentration; electrifying and preheating a detection system to keep the temperature of a detection device stable; introducing carrier gas into the mixed gas preparation device, and enabling the carrier gas to flow through the detection device to obtain a first detection value which is used as a background value of the detection system; introducing standard gas and carrier gas of perfluorinated hexanone into the mixed gas preparation device, enabling mixed gas with different proportions to flow through the detection device, respectively obtaining second detection values, and drawing a calibration curve of perfluorinated hexanone concentration; and (3) introducing a perfluorinated hexanone gas sample into the detection device, obtaining a third detection value, calibrating the third detection value according to a calibration curve, and calculating the concentration of the perfluorinated hexanone sample.
The perfluorinated hexanone gas concentration detection method based on the thermal conductivity principle comprises the steps of determining a background value, drawing a calibration curve and testing sample concentration, firstly electrifying and preheating a detection system, keeping the temperature of a detection device stable, and enabling a sensitive element to be under a constant temperature condition so as to reduce the influence of temperature rise of the detection device on a detection result and ensure the accuracy of the detection result; then, introducing carrier gas into the detection device to obtain the heat conductivity coefficient of the sensitive element in the carrier gas, namely, obtaining the heat conductivity coefficient of the sensitive element when the standard gas concentration of the perfluorinated hexanone is 0, and taking the heat conductivity coefficient as a background value K0 of the detection system; the concentration of the standard gas of the perfluorinated hexanone is regulated by changing the ratio of the standard gas of the perfluorinated hexanone to the carrier gas, so as to obtain second detection values of different standard gas concentrations of the perfluorinated hexanone, and then a calibration curve of the concentration of the perfluorinated hexanone is drawn according to the second detection values; and (3) introducing a perfluorinated hexanone gas sample into the detection device, obtaining a third detection value, calibrating the third detection value according to a calibration curve, and calculating the concentration of the perfluorinated hexanone sample.
Furthermore, before each test by using the detection device, carrier gas is introduced first to exhaust air in the pipeline of the detection system, then the detection system is preheated for 10min by electrifying, and after each device in the detection system is kept stable, the test is performed, so that the accuracy of the detection result is ensured.
Preferably, the carrier gas is one of high purity nitrogen, high purity argon, high purity air and high purity helium.
In one possible embodiment, as shown in FIG. 5, when the background value is determined, the third regulator valve is adjusted so that the carrier gas flows through the detection device at a flow rate of no more than 200 mL/min; repeating the measurement for at least 3 times, obtaining at least 3 first detection values, and taking the arithmetic average value of the first detection values as a background value.
In the technical scheme, the third regulating valve is regulated to regulate the flow rate of carrier gas entering the detection device, so that the detection device is ensured to have enough response time, the accuracy of the first detection value is improved, namely the accuracy of the background value is ensured; and through repeated measurement, taking the arithmetic average value of a plurality of first detection values as a background value to ensure the accuracy of the background value, and the accuracy of a subsequent perfluorinated hexanone concentration calibration curve is improved, so that the accuracy of a third detection value is improved.
As shown in fig. 5, in one possible implementation manner, when a calibration curve is drawn, the first regulating valve and the second regulating valve are regulated first, so that the mixed gas preparation device outputs mixed gas of standard gas of perfluoro-hexanone and carrier gas with concentration of 0%, 50%, 80%, 85%, 90%, 95% and 100%, respectively; then the third regulating valve is regulated to enable the mixed gas to flow through the detection device at a flow rate of not more than 200 mL/min; and repeatedly measuring the mixed gas of each concentration at least 3 times, respectively obtaining at least 3 second detection values of the mixed gas of each concentration, respectively taking an arithmetic average value, and drawing a calibration curve.
In the technical scheme, the concentration of the standard perfluorinated hexanone gas output by the gas mixing preparation device is accurately controlled by adjusting the first regulating valve and the second regulating valve; and then controlling the flow rate of the mixed gas entering the detection device by adjusting the third regulating valve, measuring for a plurality of times under each concentration, calculating the arithmetic average value of the second detection value under each concentration, and drawing a calibration curve according to the arithmetic average value of the heat conductivity coefficients under different concentrations so as to ensure the accuracy of the third detection value.
In one possible embodiment, as shown in FIG. 5, the fourth regulator valve is adjusted to flow the sample of perfluorinated hexanone gas through the detection device at a flow rate of no more than 200mL/min when the sample concentration is being tested; repeatedly measuring the perfluorinated hexanone gas sample for at least 3 times, obtaining at least 3 third detection values, taking the arithmetic average value of the third detection values as an indication value of the detection device, and then calculating the concentration of the perfluorinated hexanone sample according to a calibration curve.
In the technical scheme, the flow rate of the perfluorohexanone gas sample entering the detection device is controlled by adjusting the fourth regulating valve, the flow rate is measured for multiple times, then the arithmetic average value of the third detection value is calculated, so that the detection error is reduced, the accuracy of the third detection value is ensured, and the third detection value is calibrated according to the perfluorohexanone concentration calibration curve, so that the accurate concentration of the perfluorohexanone gas sample is obtained.
In a possible implementation mode, after the concentration of the perfluorinated hexanone sample is calculated, when the concentration of the perfluorinated hexanone sample is more than or equal to 90%, judging that the perfluorinated hexanone gas sample meets the requirements; and when the concentration of the perfluorinated hexanone sample is less than 90%, judging that the concentration of the perfluorinated hexanone does not meet the requirement.
In the technical scheme, if the concentration of the perfluorinated hexanone sample is detected to be more than or equal to 90%, the perfluorinated hexanone sample meets the requirements, and the perfluorinated hexanone sample is judged to be perfluorinated hexanone gas; if the concentration of the perfluorinated hexanone sample is detected to be less than 90%, the perfluorinated hexanone sample is not in accordance with the requirements, and the perfluorinated hexanone sample concentration is judged to be not in accordance with the requirements or the sample is not perfluorinated hexanone gas.
It will be readily appreciated by those skilled in the art that the above advantageous ways can be freely combined and superimposed without conflict.
The foregoing description of the preferred embodiment of the present invention is not intended to limit the invention to the particular form disclosed, but on the contrary, the intention is to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the invention. The foregoing is merely a preferred embodiment of the present application and it should be noted that it will be apparent to those skilled in the art that several modifications and variations can be made without departing from the technical principles of the present application, and these modifications and variations should also be regarded as the scope of the present application.
Claims (10)
1. The utility model provides a perfluoro hexanone gas concentration detecting system based on thermal conductance principle, its characterized in that, perfluoro hexanone gas concentration detecting system based on thermal conductance principle includes:
the mixed gas preparation device (10), the mixed gas preparation device (10) comprises a first inlet, a second inlet and an outlet, the first inlet is used for introducing the standard gas of the perfluorinated hexanone, the second inlet is used for introducing the carrier gas, and the mixed gas preparation device (10) is used for mixing the standard gas of the perfluorinated hexanone and the carrier gas;
a container (11) to be tested, wherein a perfluorinated hexanone gas sample is arranged in the container (11) to be tested;
the detecting device (12), detecting device (12) include first air inlet, second air inlet and gas vent, first air inlet with discharge port detachably is connected, the second air inlet with await measuring container (11) detachably is connected, be provided with sensing element (121) in detecting device (12), detecting device (12) are used for according to sensing element (121) thermal conductivity coefficient change volume under the constant temperature condition measures the concentration of gas.
2. The system for detecting the concentration of the perfluorinated hexanone gas based on the thermal conductivity principle according to claim 1, wherein the system for detecting the concentration of the perfluorinated hexanone gas based on the thermal conductivity principle further comprises:
the first regulating valve (13) is arranged on the first inlet, and the first regulating valve (13) is used for regulating the flow of the standard gas of the perfluorinated hexanone;
the second regulating valve (14) is arranged on the second inlet, and the second regulating valve (14) is used for regulating the flow of the carrier gas so as to regulate the mixing proportion of the standard gas of the perfluorinated hexanone and the carrier gas;
the air discharging port (15) is arranged on the mixed air preparation device (10), and the air discharging port (15) is used for discharging residual air in the mixed air preparation device (10).
3. The system for detecting the concentration of the perfluorinated hexanone gas based on the thermal conductivity principle according to claim 2, wherein the system for detecting the concentration of the perfluorinated hexanone gas based on the thermal conductivity principle further comprises:
a third regulating valve (16), the third regulating valve (16) is arranged on the first air inlet, and the third regulating valve (16) is used for regulating the flow rate of the air entering the detection device (12) from the air mixing preparation device (10);
and a fourth regulating valve (17), wherein the fourth regulating valve (17) is arranged on the second air inlet, and the fourth regulating valve (17) is used for regulating the flow rate of the perfluorinated hexanone gas sample entering the detection device (12).
4. The system for detecting the concentration of the perfluorinated hexanone gas based on the thermal conductivity principle according to claim 1, wherein the system is characterized in that:
the detection device (12) detects the concentration of the perfluorinated hexanone gas sample in the container (11) to be detected according to the heat conductivity coefficient variation of the sensitive element (121) in the mixed gas of the perfluorinated hexanone standard gas and the carrier gas.
5. A perfluorinated hexanone gas concentration detection system based on thermal conductivity principles according to claim 4, wherein said detection means (12) further comprises:
-a detection cell (125), the detection cell (125) being adapted to contain a gas, and the sensing element (121) being adapted to adsorb the gas within the detection cell (125);
the acquisition module (122) is used for acquiring the heat conductivity coefficient variation of the sensitive element (121) under the constant temperature condition;
the processing module (123) is used for converting the acquired thermal conductivity coefficient variation into voltage variation;
and the display module (124) is used for displaying the measurement result.
6. A method for detecting the concentration of perfluorinated hexanone gas based on a thermal conductivity principle, which is characterized in that the perfluorinated hexanone gas concentration detection system based on the thermal conductivity principle as claimed in any one of claims 1 to 5 is adopted, and the method comprises the following steps:
preheating detection system: energizing and preheating the detection system to keep the temperature of the detection device (12) stable;
determining a background value: introducing carrier gas into the mixed gas preparation device (10) to enable the carrier gas to flow through the detection device (12) to obtain a first detection value which is used as a background value of a detection system;
drawing a calibration curve: introducing standard gas of perfluorinated hexanone and carrier gas into the mixed gas preparation device (10) to enable mixed gas with different proportions to flow through the detection device (12), respectively obtaining second detection values, and drawing a calibration curve of perfluorinated hexanone concentration;
test sample concentration: and (3) introducing a perfluorinated hexanone gas sample into the detection device (12), obtaining a third detection value, calibrating the third detection value according to the calibration curve, and calculating the concentration of the perfluorinated hexanone sample.
7. The method for detecting the concentration of the perfluorinated hexanone gas based on the thermal conductivity principle according to claim 6, wherein the determining the background value further comprises:
-adjusting the third regulating valve (16) so that the carrier gas flows through the detection device (12) at a flow rate of not more than 200 mL/min;
repeating the measurement for at least 3 times, obtaining at least 3 first detection values, and taking an arithmetic average value of the first detection values as the background value.
8. The method for detecting the concentration of the perfluorinated hexanone gas based on the thermal conductivity principle according to claim 7, wherein the drawing of the calibration curve further comprises:
the first regulating valve (13) and the second regulating valve (14) are regulated to ensure that the output concentration of the mixed gas preparation device (10) is respectively 0%, 50%, 80%, 85%, 90%, 95% and 100% of mixed gas of standard gas of perfluorinated hexanone and carrier gas;
adjusting the third adjusting valve (16) to enable the mixed gas to flow through the detection device (12) at a flow rate of not more than 200 mL/min;
and repeatedly measuring the mixed gas of each concentration at least 3 times, respectively obtaining at least 3 second detection values of the mixed gas of each concentration, respectively taking arithmetic average values, and drawing the calibration curve.
9. The method for detecting the concentration of the perfluorinated hexanone gas based on the thermal conductivity principle according to claim 8, wherein the method for detecting the concentration of the sample further comprises the steps of:
adjusting the fourth adjusting valve (17) to enable the perfluorinated hexanone gas sample to flow through the detection device (12) at a flow rate of not more than 200 mL/min;
repeatedly measuring the perfluorinated hexanone gas sample for at least 3 times, obtaining at least 3 third detection values, taking the arithmetic average value of the third detection values as an indication value of the detection device (12), and then calculating the concentration of the perfluorinated hexanone sample according to the calibration curve.
10. The method for detecting the concentration of the perfluorinated hexanone gas based on the thermal conductivity principle according to claim 6, wherein after calculating the concentration of the perfluorinated hexanone sample, the method further comprises the following steps:
when the concentration of the perfluorinated hexanone sample is more than or equal to 90%, judging that the perfluorinated hexanone gas sample meets the requirements;
and when the concentration of the perfluorinated hexanone sample is less than 90%, judging that the concentration of the perfluorinated hexanone does not meet the requirement.
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| CN202311314923.XA CN117347431A (en) | 2023-10-10 | 2023-10-10 | Perfluorinated hexanone gas concentration detection system and detection method based on thermal conductivity principle |
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