CN112834562B - Device and method for detecting helium concentration in heat-conducting mixed gas - Google Patents
Device and method for detecting helium concentration in heat-conducting mixed gas Download PDFInfo
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- CN112834562B CN112834562B CN202110001537.XA CN202110001537A CN112834562B CN 112834562 B CN112834562 B CN 112834562B CN 202110001537 A CN202110001537 A CN 202110001537A CN 112834562 B CN112834562 B CN 112834562B
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- 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
Abstract
The invention relates to a device and a method for detecting helium concentration in heat-conducting mixed gas, belonging to the technical field of gas sensing; firstly, measuring the concentrations of methane, carbon dioxide, hydrogen, oxygen, water vapor and the like in the mixed gas by using a multi-component gas detector; then, inquiring and obtaining the pure material thermal conductivity of each component of the sample at a specific temperature, and calculating the thermal conductivity generated by gas with known concentration by using the measured concentration and the thermal conductivity thereof; controlling the thermal conductivity sensing probe to a preset temperature by using a first temperature control device, and calibrating the sum of the thermal conductivity of 80% nitrogen and the thermal conductivity of gas with known concentration as a 'zero point' of the thermal conductivity sensing probe; the temperature of the mixed gas is regulated and controlled by using a second temperature control device, the output voltage of the probe of the thermal conductivity sensor is read, the thermal conductivity of the unknown component minus the thermal conductivity of 80% of nitrogen is taken as the detection signal of the probe of the thermal conductivity sensor to be in direct proportion to the output voltage, and the helium concentration is obtained by using the simultaneous equation system of the relation of the specific temperature.
Description
Technical Field
The invention belongs to the technical field of gas sensing, and particularly relates to a device and a method for detecting helium concentration in heat-conducting mixed gas.
Background
Earthquake is a phenomenon that the medium inside the earth is locally and rapidly broken to generate earthquake waves, so that ground vibration is caused in a certain range, and great loss is caused to the life and property safety of people due to earthquake disasters. In a period of time before earthquake, deep earth gas containing a large amount of geological information overflows the earth surface along a fracture zone, and accurate detection of the gas is an effective earthquake early warning means, and especially has great significance on helium concentration detection with stable properties.
At present, helium concentration detection is mainly based on a mass spectrometry technology, a gas chromatography technology and a thermal conductivity gas sensing technology. The mass spectrometry has high detection accuracy and low detection limit, is the main mode for detecting the helium gas concentration at present, but has the defects of high cost, large volume, complex structure and high vacuum (the vacuum degree is lower than 10)-6) Under the conditions of (1) feeding the sampleAnd (5) line preprocessing. The gas chromatography technology is suitable for multi-component detection, has the characteristic of high detection precision, but needs carrier gas and ensures carrier gas pressure and flow velocity simultaneously in the using process, and chromatographic columns need to be replaced regularly, and also has the characteristics of complex structure and high cost. These factors greatly limit the application of mass spectrometry and chromatography in the field of geochemical exploration.
The heat conduction gas sensing technology has the characteristics of small volume and low cost, and is popular with scholars at home and abroad. At present, the thermal conductivity gas sensing can accurately detect the helium concentration under the condition of detecting the unchanged background gas, the helium in the background gas can not be distinguished due to the thermal conductivity of the gas to be detected by the thermal conductivity gas sensing technology, and the helium concentration detection can not be realized when the components of the background gas change.
In summary, how to realize helium concentration detection with convenient measurement, low cost, good stability and high sensitivity is one of the important subjects in the field of geochemical detection.
Disclosure of Invention
The invention aims to provide a device and a method for detecting helium concentration in heat conduction type mixed gas, aiming at the problems that in the prior art, when a heat conduction sensor probe measures helium concentration, cross sensitivity exists, and the background gas concentration changes to change a base line of the heat conduction sensor probe, so that measurement is inaccurate, and even helium concentration cannot be measured.
The purpose of the invention is realized by the following technical scheme: a device and method for detecting helium concentration in heat conduction type mixed gas are characterized by comprising the following steps which are sequentially carried out:
a helium concentration detection device in heat-conduction multi-component mixed gas comprises a multi-component gas detector and a microcomputer, wherein the multi-component gas detector is connected with a sample absorption cell through a first valve;
the outer surface of the sample absorption pool is provided with a second temperature sensor, the interior of the sample absorption pool is provided with a first temperature control device, a heat conduction sensor probe is arranged in the first temperature control device, and the surface of the heat conduction sensor probe is provided with a plurality of first temperature sensors;
the sample absorption cell is connected with a vacuum pump through a second valve;
a second temperature control device is arranged outside the sample absorption cell, the second valve and the vacuum pump;
one end of the microcomputer is electrically connected with the thermal conductivity sensor probe, the first temperature sensor and the second temperature sensor through the acquisition circuit, and the other end of the microcomputer is electrically connected with the first temperature control device and the second temperature control device through the control circuit.
A helium concentration detection method in a heat conduction type multi-element mixed gas comprises the following steps, and the steps are sequentially carried out:
step 1: measuring the concentrations of methane, carbon dioxide, hydrogen, oxygen and water vapor in the mixed gas by using a high-precision gas detection system, and respectively marking the concentrations as
Step 2: the thermal conductivity of all component pure substances in the mixed gas at a specific temperature is obtained by inquiring a database
λHe(Ti)、
λAr(Ti)、λNe(Ti)、λKr(Ti) Etc. according to the concentration of methane, carbon dioxide, hydrogen, oxygen, water vapor measured in said step 1
And the inquired thermal conductivity of methane, carbon dioxide, water, hydrogen and oxygen, and calculating the thermal conductivity K of the gas with the known concentration1(Ti)，K1(Ti) The formula is as follows:
and step 3: according to the temperature measured by the first temperature sensor, the probe of the thermal conductivity sensor is regulated to a preset temperature by using the first temperature control device, then the probe of the thermal conductivity sensor is calibrated, and the thermal conductivity K of the gas with the known concentration is measured1(Ti) And the sum of the thermal conductivity of 80% nitrogen is marked as the output zero point of the thermal conductivity sensor probe;
and 4, step 4: filling the mixture into a sample absorption cell, and accurately regulating the temperature of the sample absorption cell to T by using a second temperature control device according to the temperature measured by a second temperature sensoriAnd after stabilizing for 10 minutes, the gas temperature reaches the temperature T of the sample absorption celliReading the output voltage V of the thermal conductivity sensor probeiI equals the unknown gas quantity;
and 5: subtracting 80% of nitrogen thermal conductivity from the thermal conductivity of the unknown component to obtain the gas thermal conductivity detected by the thermal conductivity sensor probe, wherein the detected gas thermal conductivity is in direct proportion to the output voltage of the thermal conductivity sensor probe, and the pure material thermal conductivity and the output voltage of the thermal conductivity sensor probe inquired in the step 2 are utilized to establish a simultaneous equation set at different specific temperatures, and the equation set is solved to obtain the concentration C of helium in the multi-component mixed gasHe。
Further, in the step 3, in the process of regulating and controlling the probe of the thermal conductivity sensor to the preset temperature by using the first temperature control device, the method for measuring the temperature of the probe of the thermal conductivity sensor comprises the following steps: the temperature sensors are arranged at four positions of the outer surface of the probe of the thermal conductivity sensor, namely the upper position, the lower position, the left position and the right position, and are used for measuring the temperature T of the probe of the thermal conductivity sensor1、T2、T3、T4When the temperatures of the thermal conductivity sensor probe are equal at the respective positions, i.e. T1、T2、T3、T4When they are equal, the thermal conductivity sensor probe is considered to reach the preset temperature.
Further, in the step 4, in the process of measuring the thermal conductivity of the mixture, the total amount of the mixture in the sample absorption cell needs to be ensured to be unchanged, a static measurement mode is adopted in the measurement process, the first valve, the second valve and the vacuum pump are immediately closed after the sample is introduced for the first time, and meanwhile, the airtightness of the sample absorption cell is ensured to avoid the interference of the external gas entering the sample absorption cell on the measurement.
Further, in the step 4, the method for detecting the temperature of the sample absorption cell includes: selecting 1 temperature measuring point on the outer surface of the sample absorption pool of the mixture, measuring the temperature of the temperature measuring point by using a second temperature sensor, and obtaining the characteristic temperature T of the mixture after a period of time after the temperature of the temperature measuring point is stable, wherein the characteristic temperature T of the mixture is the temperature of the outer surface of the sample absorption pool when the thermal conductivity value of the mixture is measured.
Further, in step 5, the difference between the thermal conductivity of the component gas with unknown concentration and the thermal conductivity of 80% nitrogen is equal to the output voltage of the thermal conductivity sensor probe, and can be represented by the following formula:
and (4) simultaneously solving to obtain the concentration of helium in the multi-component mixture.
The device and the method for detecting the helium concentration in the heat conduction type mixed gas have the following advantages that: the method can realize the rapid detection of the helium concentration in the mixed gas by utilizing the heat conduction gas sensor and combining with a multi-component gas detector, specifically, the heat conductivity of a mixture under different specific temperature conditions is measured according to different change rates of different gas heat conductivities to temperature, the heat conductivity of the gas with the known concentration and the heat conductivity of 80% nitrogen at constant temperature are used as a zero line of a heat conduction sensor probe, and the heat conductivity of unknown components at different temperatures and the output of the heat conduction sensor probe are simultaneously solved, so that the helium concentration can be obtained.
Drawings
Fig. 1 is a block diagram of a device for detecting helium concentration in a thermally conductive mixed gas and a device structure adopted by the method in the embodiment of the present invention.
Fig. 2 is a detection flowchart of a device and a method for detecting helium concentration in a thermally conductive mixed gas according to the present invention.
The notation in the figure is: 1. a multi-component gas detector; 2. a microcomputer; 3. a first valve; 4. a sample absorption cell; 5. a thermal conductivity sensor probe; 6. a first temperature sensor; 7. a first temperature control device; 8. a second valve; 9. a vacuum pump; 10. a second temperature control device; 11. an air inlet; 12. an acquisition circuit; 13. a control circuit; 14. a second temperature sensor.
Detailed Description
In order to better understand the purpose, structure and function of the present invention, the following describes the device and method for detecting helium concentration in a heat-conducting mixed gas in detail with reference to the accompanying drawings.
As shown in fig. 1, a device for detecting helium concentration in a thermally conductive multi-component mixed gas comprises a multi-component gas detector 1 and a microcomputer 2, wherein the multi-component gas detector 1 is connected with a sample absorption cell 4 through a first valve 3;
a second temperature sensor 14 is arranged on the outer surface of the sample absorption cell 4, a first temperature control device 7 is arranged in the sample absorption cell, a thermal conductivity sensor probe 5 is arranged in the first temperature control device 7, and a plurality of first temperature sensors 6 are arranged on the surface of the thermal conductivity sensor probe 5; the thermal conductivity gas sensing technology is quite mature, but the detection precision is easily influenced by temperature change, and the first temperature control device 7 is utilized to maintain the probe 5 of the thermal conductivity sensor and the first temperature sensor 6 in a constant temperature state so as to ensure the detection precision;
the sample absorption cell 4 is connected with a vacuum pump 9 through a second valve 8;
a second temperature control device 10 is arranged outside the sample absorption cell, the second valve 8 and the vacuum pump 9;
one end of the microcomputer 2 is electrically connected with the thermal conductivity sensor probe 5, the first temperature sensor 6 and the second temperature sensor 14 through the acquisition circuit 12, and the other end is electrically connected with the first temperature control device 7 and the second temperature control device 10 through the control circuit 13.
The microcomputer 2 controls the probe 5 of the thermal conductivity sensor and the first temperature control device 7 to preheat, when the sample absorption cell 4 reaches a preset temperature, the first valve 3, the second valve 8 and the vacuum pump 9 are opened to charge the mixture sample, the temperature of the sample absorption cell 4 is changed, and data is processed to obtain helium concentration analysis in the multi-component mixture;
the multi-component gas detector 1 is used for detecting the concentration of gas such as methane, carbon dioxide, hydrogen, oxygen, water vapor and the like;
the acquisition circuit 12 acquires a detection signal with component concentration information and stores the detection signal into the microcomputer 2; meanwhile, the thermal conductivity of the samples with different specific temperatures is also stored in the computer, the measurement signal of the thermal conductivity sensor probe 5, the thermal conductivity of each component and the concentration of the detected known gas are used for calculation, and the helium concentration in the multi-component mixture is obtained, wherein the specific detection process is shown in fig. 2.
Mixed with standard gas (40000ppmv CH)4，50000ppmv CO2,10000ppmv He，90％N2) The method for detecting the helium concentration in the heat-conducting multi-element mixed gas, which is provided by the invention, is used as an example, and the implementation process of the method for detecting the helium concentration in the heat-conducting multi-element mixed gas comprises the following steps which are sequentially carried out:
step 1: measuring the concentration of methane and carbon dioxide in the mixed standard gas by using a methane and carbon dioxide gas detection system
The results of the detection of the concentrations of the methane gas and the carbon dioxide gas are 40015ppmv and 49960ppmv respectively.
Step 2: obtaining pure material thermal conductivities of methane, carbon dioxide, nitrogen and helium at 25 ℃ and 35 ℃ by querying a database:
λHe(25)＝0.1553W/(m·K)；
λHe(35)＝0.1589W/(m·K)；
calculating the thermal conductivity K of the methane and the carbon dioxide gas by using a formula (1) according to the concentration 40015ppmv of the methane gas and the concentration 49960ppmv of the carbon dioxide gas measured in the step 1 and the inquired thermal conductivity of the methane and the carbon dioxide1(25) And K1(35) 0.00136W/(m.K) and 0.00142W/(m.K) respectively;
and step 3: regulating and controlling the thermal conductivity sensor probe 5 to a preset temperature, and specifically, controlling the thermal conductivity sensor probe 5 to 25 ℃ by using a first temperature control device 7 according to the temperature measured by a first temperature sensor 6, calibrating the thermal conductivity sensor probe 5, and taking the sum of the thermal conductivity of nitrogen with the concentration of 80% and the thermal conductivity of methane and carbon dioxide gas as a zero point of the thermal conductivity sensor probe 5;
and 4, step 4: and (3) filling the mixed standard gas into the sample absorption cell, regulating and controlling the temperature of the sample absorption cell to 25 ℃ by using a second temperature control device 10 according to the temperature measured by a second temperature sensor 14, stabilizing the temperature of the gas for 10 minutes until the temperature of the sample absorption cell reaches 25 ℃, reading the output voltage of the thermal conductivity sensor probe 5 to be 4213.00mV, heating the sample absorption cell to 35 ℃ by using the second temperature control device 10, and reading the output voltage of the thermal conductivity sensor probe 5 to be 4319.01mV after stabilizing the temperature for 10 minutes.
And 5: the output result of the thermal conductivity sensor probe 5 is that the thermal conductivity of the unknown gas subtracts 80% of the thermal conductivity of nitrogen, and the helium concentration in the mixed standard gas is calculated by using the formula (2), the thermal conductivity of pure substances of methane and carbon dioxide gas inquired in the step 2 and the measured voltages of the thermal conductivity sensor probe 5 at 25 ℃ and 35 ℃ calculated in the step 5, and can be represented by the following formula:
solving the equation set gave a helium concentration of 9980ppmv in the mixing standard, which was 20ppmv different from the actual standard gas concentration.
It is to be understood that the present invention has been described with reference to certain embodiments, and that various changes in the features and embodiments, or equivalent substitutions may be made therein by those skilled in the art without departing from the spirit and scope of the invention. In addition, many modifications may be made to adapt a particular situation or material to the teachings of the invention without departing from the essential scope thereof. Therefore, it is intended that the invention not be limited to the particular embodiment disclosed, but that the invention will include all embodiments falling within the scope of the appended claims.
Claims (5)
1. A method for detecting the helium concentration in a heat-conducting mixed gas is characterized by comprising the following steps which are sequentially carried out:
step 1: measuring the concentrations of methane, carbon dioxide, hydrogen, oxygen and water vapor in the mixed gas by using a high-precision gas detection system, and respectively marking the concentrations as
Step 2: the thermal conductivity of all component pure substances in the mixed gas at a specific temperature is obtained by inquiring a database
According to the concentration of methane, carbon dioxide, hydrogen, oxygen and water vapor measured in the step 1
And the inquired thermal conductivity of methane, carbon dioxide, water, hydrogen and oxygen, and calculating the thermal conductivity K of the gas with the known concentration1(Ti)，K1(Ti) The formula is as follows:
and step 3: according to the temperature measured by the first temperature sensor (6), the first temperature control device (7) is utilized to regulate and control the thermal conductivity sensor probe (5) to a preset temperature, then the thermal conductivity sensor probe (5) is calibrated, and the thermal conductivity K of the gas with the known concentration is measured1(Ti) And the sum of the thermal conductivity of 80% nitrogen is marked as the output zero point of the thermal conductivity sensor probe (5);
and 4, step 4: the mixture is filled into a sample absorption cell (4), and the temperature of the sample absorption cell (4) is accurately regulated to T by utilizing a second temperature control device (10) according to the temperature measured by a second temperature sensor (14)iThe gas temperature reaches the temperature T of the sample absorption cell (4) after being stabilized for 10 minutesiReading the output voltage V of the thermal conductivity sensor probe (5)iI equals the unknown gas quantity;
and 5: subtracting 80% of nitrogen thermal conductivity from the thermal conductivity of the unknown component to obtain the gas thermal conductivity detected by the thermal conductivity sensor probe (5), wherein the detected gas thermal conductivity is in direct proportion to the output voltage of the thermal conductivity sensor probe (5), simultaneous equation sets are carried out at different specific temperatures by using the pure material thermal conductivity inquired in the step 2 and the output voltage of the thermal conductivity sensor probe (5), and the concentration C of helium in the multi-component mixed gas can be obtained by solving the equation setsHe；
The device used in the method for detecting the helium concentration in the heat-conducting mixed gas comprises a multi-component gas detector (1) and a microcomputer (2), wherein the multi-component gas detector (1) is connected with a sample absorption cell (4) through a first valve (3);
a second temperature sensor (14) is arranged on the outer surface of the sample absorption cell (4), a first temperature control device (7) is arranged in the sample absorption cell, a thermal conductivity sensor probe (5) is arranged in the first temperature control device (7), and a plurality of first temperature sensors (6) are arranged on the surface of the thermal conductivity sensor probe (5);
the sample absorption cell (4) is connected with a vacuum pump (9) through a second valve (8);
a second temperature control device (10) is arranged outside the sample absorption cell (4), the second valve (8) and the vacuum pump (9);
one end of the microcomputer (2) is electrically connected with the thermal conductivity sensor probe (5), the first temperature sensor (6) and the second temperature sensor (14) through the acquisition circuit (12), and the other end of the microcomputer is electrically connected with the first temperature control device (7) and the second temperature control device (10) through the control circuit (13).
2. The method for detecting the helium concentration in the thermally conductive mixed gas as claimed in claim 1, wherein in the step 3, the first temperature control device (7) is used to control the thermal conductivity sensor probe (5) to a preset temperature, and the method for measuring the temperature of the thermal conductivity sensor probe (5) comprises: temperature sensors are arranged at four positions of the upper, lower, left and right of the outer surface of the thermal conductivity sensor probe (5) to measure the temperature T of the thermal conductivity sensor probe (5)1、T2、T3、T4When the temperatures of all the positions of the thermal conductivity sensor probe (5) are equal, namely T1、T2、T3、T4When the temperature is equal, the thermal conductivity sensor probe (5) is considered to reach the preset temperature.
3. The method for detecting the helium concentration in a thermally conductive mixed gas as claimed in claim 1, wherein in the step 4, during the measurement of the thermal conductivity of the mixture, it is required to ensure that the total amount of the mixture in the sample absorption cell (4) is not changed, a static measurement method is adopted during the measurement, the first valve (3), the second valve (8) and the vacuum pump (9) are closed immediately after the first sample introduction, and meanwhile, the airtightness of the sample absorption cell (4) is ensured to prevent the external gas from entering the sample absorption cell (4) to interfere the measurement.
4. The method of claim 1, wherein the step 4 comprises detecting the temperature of the sample cell by: selecting 1 temperature measuring point on the outer surface of the mixture sample absorption tank (4), measuring the temperature of the temperature measuring point by using a second temperature sensor (14), and obtaining the characteristic temperature T of the mixture after a period of time after the temperature of the temperature measuring point is stable, wherein the characteristic temperature T of the mixture is the outer surface temperature of the sample absorption tank (4) when the thermal conductivity value of the mixture is measured.
5. The method of claim 1, wherein in step 5, the difference between the thermal conductivity of the component gas with unknown concentration and the thermal conductivity of 80% nitrogen gas is equal to the output voltage of the thermal conductivity sensor probe (5) and is expressed by the following formula:
and (4) simultaneously solving to obtain the concentration of helium in the multi-component mixture.
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