CN107389498B - Method for measuring methane transmittance - Google Patents
Method for measuring methane transmittance Download PDFInfo
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- CN107389498B CN107389498B CN201710589542.0A CN201710589542A CN107389498B CN 107389498 B CN107389498 B CN 107389498B CN 201710589542 A CN201710589542 A CN 201710589542A CN 107389498 B CN107389498 B CN 107389498B
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 238000002834 transmittance Methods 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title claims abstract description 17
- 238000012360 testing method Methods 0.000 claims abstract description 88
- 239000007789 gas Substances 0.000 claims abstract description 84
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims abstract description 63
- 239000001307 helium Substances 0.000 claims abstract description 59
- 229910052734 helium Inorganic materials 0.000 claims abstract description 59
- 238000001819 mass spectrum Methods 0.000 claims abstract description 29
- 239000000523 sample Substances 0.000 claims description 102
- 238000005259 measurement Methods 0.000 claims description 10
- 230000035699 permeability Effects 0.000 claims description 9
- 238000007789 sealing Methods 0.000 claims description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical group [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- 239000003292 glue Substances 0.000 claims 1
- 210000003437 trachea Anatomy 0.000 claims 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000000149 penetrating effect Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004949 mass spectrometry Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N7/00—Analysing materials by measuring the pressure or volume of a gas or vapour
- G01N7/10—Analysing materials by measuring the pressure or volume of a gas or vapour by allowing diffusion of components through a porous wall and measuring a pressure or volume difference
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
Abstract
The invention relates to the field of gas transmittance testing, in particular to a method for measuring methane transmittance, which comprises the steps of opening a pneumatic valve, taking a sample frame to a sample transferring cavity, opening a valve I and a valve II, and vacuumizing a device by a vacuum pump; closing a pneumatic valve and a valve I, opening a helium micro-leakage device to enable helium to enter a test cavity after passing through a gate valve at a constant leakage rate, and starting a mass spectrum to start a calibration process; after the system is stable, a relation curve between the vacuum degree and the helium leakage rate and a relation curve between the helium partial pressure and the helium leakage rate are obtained; measuring the helium partial pressure of the high-pressure area and the helium partial pressure of the test area, and estimating effusion from the known helium partial pressures under the condition of a certain leak rate; calculating the collision rate of helium atoms with the surface of the unit area in unit time; closing the helium micro-leakage device and the valve II, taking the sample frame to a test cavity, opening the gas storage tank and the valve I, testing the transmittance of methane, and obtaining the methane partial pressure of a high-pressure area and a test area; the transmittance of methane in the sample was calculated.
Description
Technical Field
The invention relates to the field of gas transmittance testing, in particular to a method for measuring methane transmittance, which can improve measurement accuracy and calibrate different gases.
Background
In the existing method for measuring the gas permeability (transmission rate), such as a method for measuring the gas permeability by using mass spectrometry, a mass flowmeter is generally used in the prior art to measure the amount of the introduced gas, the accuracy is low, in the case of samples with very low gas permeability, such as the permeation of methane gas in certain industrial organic protective films, the test usually needs a long time, thus large errors are caused, in addition, the dynamic volume of methane molecules is usually different from helium, nitrogen and other gases with relatively stable chemical properties, which causes larger errors in the measurement of the mass flowmeter and data accuracy to be reduced, and the method for measuring the methane permeability can solve the problems.
Disclosure of Invention
In order to solve the problems, the invention uses the calibrated helium micro-leakage device to calibrate the gas transmittance, improves the measurement accuracy, and has a specially designed gate valve to calibrate different gases.
The technical scheme adopted by the invention is as follows:
the method for measuring the methane transmittance mainly comprises a helium micro-leakage device, a gas storage tank, a barometer, a valve I, a valve II, a gate valve, a sample transferring cavity, a sample transferring rod, a pneumatic valve, a high-pressure area, a sample rack, a test area, a mass spectrum, a test cavity, a vacuum pump and a gas pipe, wherein the high-pressure area, the sample rack and the test area are all positioned in the test cavity, the sample rack can divide the test cavity into the high-pressure area and the test area when being mounted in the test cavity, the center of the sample rack is provided with a penetrating opening, the opening is the only gas path between the high-pressure area and the test area when the sample rack is mounted in the test cavity, the outer end of the test area is provided with the mass spectrum, the mass spectrum inlet is positioned in the test area, the sample is glued on one surface of the sample rack and is positioned in the high-pressure area and completely covers the opening in the center of the sample rack, the sample transferring cavity is connected with the test cavity through the pneumatic valve, and the sample transferring cavity is provided with the sample transferring rod and the sample transferring cavity can be connected between the sample transferring cavity and the test cavity and the sample transferring pump; the leakage rate of helium in the helium micro-leakage device is controllable at a certain temperature and calibrated, methane gas is stored in the gas storage tank, valves are arranged at the outlets of the helium micro-leakage device and the gas storage tank, the helium micro-leakage device is connected with the gas storage tank through a gas pipe, a residual gas analyzer is arranged at the connection position of the gas pipe, then the gas pipe is respectively connected with a gas circuit I and a gas circuit II, the gas pipe is connected to a high-pressure area of the test cavity, the gas circuit I is sequentially connected with the valves II and a gate valve, the gas circuit II is provided with the valves I, a plurality of baffles are arranged in the gate valve, holes with different sizes are respectively arranged in the baffles, so that the cross section area of the gas circuit is changed, a residual gas analyzer is arranged in the high-pressure area and the test area, the diameter of the holes in the gate valve is 30 micrometers to 150 micrometers, the distance from the inlet to a sample is 20 micrometers to 50 micrometers, the diameter of the sample is 1 millimeter to the center of the sample, the capillary is 1 millimeter to the diameter of the sample is 1 millimeter, and the diameter of the sample is 1 millimeter to the sample is the sealing frame is 1 millimeter, and the sealing frame is in the shape is the sealing frame is the shape of the sealing frame is the diameter of the sample is 1 millimeter.
The method for measuring the methane transmittance comprises the following steps:
opening the pneumatic valve, taking the sample rack to the sample transferring cavity by using the sample transferring rod, opening the valve I and the valve II, and opening the vacuum pump to vacuumize the device;
closing the pneumatic valve, closing the valve I, opening the helium micro-leakage device to enable helium to enter the test cavity after passing through the gate valve at a constant leakage rate, and starting the mass spectrum to start a calibration process;
thirdly, after the system is stable, a relation curve between the vacuum degree and the helium leakage rate and a relation curve between the helium partial pressure and the helium leakage rate are obtained;
measuring the helium partial pressure of the high-pressure area and the helium partial pressure of the test area, estimating effusion according to the known helium partial pressure under the condition of a certain leak rate, and recording the ion current of the mass spectrum to obtain a relation curve of the ion current of the mass spectrum and the effusion;
fifthly, calculating the collision rate of helium atoms with the surface of unit area in unit timeThat is, the number of collisions per unit area per unit time, where p is the gas pressure, m is the molecular mass, k is the boltzmann constant, T is the temperature, and the gate valve baffle open area is obtained from the effusion ratio obtained in step four;
closing the helium micro-leakage device, closing the valve II, taking the sample rack to the test cavity by using the sample conveying rod, separating the test cavity into the high-pressure area and the test area, opening the gas storage tank, opening the valve I, performing a transmittance test on methane, comparing the ion current obtained by the mass spectrum with a relation curve of the ion current of the mass spectrum obtained by the step IV and the effusion of helium, and calibrating the partial pressure of the methane in the high-pressure area and the test area obtained by measurement;
seventh calculating the leakage rate of methane from the high pressure zone to the test zone at the sampleWherein A is the open area of the gate valve baffle plate and P obtained in the step five 1 And P 2 Respectively obtaining the partial pressure of methane in the high-pressure area and the test area after calibration in the step six, d is the thickness of the sample, and Q is the permeability coefficient of methane in the sample material;
and eighthly, multiplying the leak rate of the methane at the sample obtained in the step seven by the partial pressure of the methane in the test area to obtain the transmittance of the methane in the sample.
The beneficial effects of the invention are as follows:
according to the fact that the average free path of different gas molecules is different under different air pressure conditions, and the pumping speed of the vacuum pump is different for the different gas molecules, the gate valve specially designed in the invention can provide different cross sectional areas of the air paths, so that the air flow can be stable under different air pressure conditions for different gases; the invention uses the calibrated helium micro-leakage device to calibrate the gas permeability, improves the measurement precision, can complete the calibration and measurement at one time, and has a specially designed gate valve, so that different gases can be calibrated without opening a vacuum system of the device.
Drawings
The following is further described in connection with the figures of the present invention:
FIG. 1 is a schematic diagram of the present invention.
In the figure, 1, a helium micro-leakage device, 2, a gas storage tank, 3, a barometer, 4, a valve I,5, a valve II,6, a gate valve, 7, a sample conveying cavity, 8, a sample conveying rod, 9, a pneumatic valve, 10, a high-pressure area, 11, a sample, 12, a sample rack, 13, a test area, 14, a mass spectrum, 15, a test cavity and 16, a vacuum pump.
Detailed Description
As shown in fig. 1, the measuring device mainly comprises a helium micro-leakage device 1, a gas storage tank 2, a barometer 3, a valve I4, a valve II5, a gate valve 6, a sample transferring cavity 7, a sample transferring rod 8, a pneumatic valve 9, a high-pressure area 10, a sample 11, a sample rack 12, a test area 13, a mass spectrum 14, a test cavity 15, a vacuum pump 16 and a gas pipe, wherein the high-pressure area 10, the sample 11, the sample rack 12 and the test area 13 are all positioned in the test cavity 15, the sample rack 12 can divide the test cavity 15 into the high-pressure area 10 and the test area 13 when being installed in the test cavity 15, the center of the sample rack 12 is provided with an opening penetrating through, when the sample rack 12 is installed in the test cavity 15, the opening is the only gas path between the high-pressure area 10 and the test area 13, the outer end of the test area 13 is provided with the mass spectrum 14, the inlet of the mass spectrum 14 is positioned in the test area 13, the sample 11 is glued on one surface of the sample rack 12 by vacuum, the sample rack 12 is positioned on one surface 10 and covers the high-pressure area 10, the sample rack 12 completely covers the sample rack 12 and the sample transferring cavity 7 and the sample cavity 15 is connected with the sample transferring cavity 7 and the sample transferring cavity 15 through the pneumatic valve 15, and the sample rack 7 is connected with the sample transferring cavity 7 and the sample cavity 15 is connected with the sample cavity 7; the leakage rate of helium in the helium micro-leakage device 1 is controllable at a certain temperature and calibrated, the methane gas is stored in the gas storage tank 2, valves are arranged at the outlets of the helium micro-leakage device 1 and the gas storage tank 2, the helium micro-leakage device 1 and the gas storage tank 2 are connected through a gas pipe, the gas meter 3 is arranged at the joint of the gas pipe, then the gas pipe is respectively connected with a gas circuit I and a gas circuit II through the gas pipe, the gas circuit I is connected with the high-pressure area 10 of the test cavity 15, the gas circuit I is sequentially connected with the valve II5 and the gate valve 6, the gas circuit II is provided with the valve I4, a plurality of baffles are arranged inside the gate valve 6, holes with different sizes are respectively arranged on different baffles, and the vacuum environment can not be damaged, the gas paths in the different baffle plates are used for blocking the gas paths so as to change the cross-sectional area of the gas paths, residual gas analyzers are arranged in the high-pressure area 10 and the test area 13 and used for measuring gas partial pressure, the diameter of a hole in the baffle plate in the gate valve 6 is 30 micrometers to 150 micrometers, the distance from the inlet of the mass spectrum 14 to the sample 11 is 20 millimeters to 50 millimeters, the inlet of the mass spectrum 14 is in a capillary shape and has a length of 5 millimeters to 30 millimeters and an inner diameter of 0.3 millimeters to 1 millimeter, the opening shape in the center of the sample frame 12 is a round shape with a diameter of 1 millimeter to 5 millimeters or a square with a side length of 1 millimeter to 3 millimeters, the thickness of the sample 11 is 200 micrometers to 2 millimeters, and the sealing structure of the sample frame 12 and the test cavity 15 is a rubber ring seal or a copper ring seal.
The method for measuring the methane transmittance comprises the following steps:
firstly, opening the pneumatic valve 9, taking the sample frame 12 to the sample transferring cavity 7 by using the sample transferring rod 8, opening the valve I4 and the valve II5, and opening the vacuum pump 16 to vacuumize the device;
closing the pneumatic valve 9, closing the valve I4, opening the helium micro-leakage device 1, enabling helium to enter the test cavity 15 after passing through the gate valve 6 at a constant leakage rate, opening the mass spectrum 14, and starting a calibration process;
thirdly, after the system is stable, a relation curve between the vacuum degree and the helium leakage rate and a relation curve between the helium partial pressure and the helium leakage rate are obtained;
measuring the helium partial pressure of the high-pressure area 10 and the helium partial pressure of the test area 13, estimating effusion from the known helium partial pressure under the condition of a certain leak rate, and recording the ion current of the mass spectrum 14 to obtain a relation curve of the ion current of the mass spectrum and the effusion;
fifthly, calculating the collision rate of helium atoms with the surface of unit area in unit timeThat is, the number of collisions per unit area per unit time, where p is the gas pressure, m is the molecular mass, k is the boltzmann constant, T is the temperature, and the open area of the shutter 6 is obtained from the effusion ratio obtained in the fourth step;
closing the helium micro-leakage device 1, closing the valve II5, taking the sample rack 12 to the test cavity 15 by using the sample conveying rod 8, separating the test cavity 15 into the high-pressure area 10 and the test area 13, opening the gas storage tank 2, opening the valve I4, performing a transmittance test on methane, comparing an ion current obtained by the mass spectrum 14 with a relation curve of the ion current of the mass spectrum obtained by the step four and the effusion of helium, and calibrating partial pressures of the methane in the high-pressure area 10 and the test area 13 obtained by measurement;
seventh calculating the leakage rate of methane from the high pressure zone 10 to the test zone 13 at the sampleWherein A is the open area of the baffle plate of the gate valve 6 obtained in the fifth step, P 1 And P 2 The partial pressure of methane in the high-pressure area 10 and the test area 13 after calibration obtained in the step six, d is the thickness of the sample 11, and Q is the permeability coefficient of methane in the sample material;
and eighthly, multiplying the leak rate of the methane at the sample obtained in the step seven by the partial pressure of the methane in the test area 13 to obtain the transmittance of the methane in the sample 11.
The invention uses the calibrated helium micro-leakage device to calibrate the gas permeability, improves the measurement precision, can complete the calibration and measurement at one time, and has a specially designed gate valve, so that different gases can be calibrated without opening a vacuum system of the device.
Claims (1)
1. The utility model provides a method for measuring methane transmissivity, measuring device mainly includes helium micro-leak device (1), gas holder (2), barometer (3), valve I (4), valve II (5), flashboard valve (6), pass appearance chamber (7), pass appearance pole (8), pneumatic valve (9), high-pressure region (10), sample (11), sample frame (12), test area (13), mass spectrum (14), test chamber (15), vacuum pump (16) and trachea, high-pressure region (10), sample (11), sample frame (12), test area (13) all are located in test chamber (15), can separate test chamber (15) into high-pressure region (10) and test area (13) when sample frame (12) is installed test chamber (15), sample frame (12) center has the opening that runs through, when sample frame (12) is installed test chamber (15), the opening is high-pressure region (10) and test area (13) between, test area (13) are located in test chamber (15), test area (13) are installed to test end (14) are installed in mass spectrum area (13), the sample (11) is adhered to one surface of the sample frame (12) located in the high-pressure area (10) by vacuum glue, and completely covers an opening in the center of the sample frame (12), the sample transferring cavity (7) is connected with the test cavity (15) through the pneumatic valve (9), the sample transferring cavity (7) is provided with the sample transferring rod (8) and can transfer the sample frame (12) between the sample transferring cavity (7) and the test cavity (15), and the test cavity (15) is connected with the vacuum pump (16); the leakage rate of helium in the helium micro-leakage device (1) is controllable at a certain temperature and calibrated, methane gas is stored in the gas storage tank (2), valves are arranged at the outlets of the helium micro-leakage device (1) and the gas storage tank (2), the helium micro-leakage device (1) and the gas storage tank (2) are connected through a gas pipe, the gas meter (3) is arranged at the joint of the gas pipe, then a gas circuit I and a gas circuit II are respectively connected through the gas pipe, the gas circuit I is connected to the high-pressure area (10) of the test cavity (15), the gas circuit I is sequentially connected with the valve II (5) and the gate valve (6), the valve I (4) is arranged on the gas circuit II, a plurality of baffles are arranged inside the gate valve (6), the different baffles are respectively provided with holes with different sizes, the gas paths in the devices can be blocked by the different baffles under the condition of not damaging the vacuum environment so as to change the cross section area of the gas paths, the high-pressure area (10) and the test area (13) are respectively internally provided with a residual gas analyzer for measuring the partial pressure of gas, the diameter of the holes on the inner baffle of the flashboard valve (6) is 30 micrometers to 150 micrometers, the distance from an inlet of a mass spectrum (14) to a sample (11) is 20 millimeters to 50 millimeters, the inlet of the mass spectrum (14) is in a capillary shape and has the length of 5 millimeters to 30 millimeters and the inner diameter of 0.3 millimeter to 1 millimeter, and the opening shape of the center of the sample frame (12) is in a round shape with the diameter of 1 millimeter to 5 millimeters, or square with side length of 1 mm to 3 mm, wherein the thickness of the sample (11) is 200 micrometers to 2 mm, the sealing structure of the sample frame (12) and the test cavity (15) is rubber ring sealing or copper ring sealing,
the method is characterized in that: the method for measuring the methane transmittance comprises the following steps:
opening the pneumatic valve (9), taking the sample rack (12) to the sample transferring cavity (7) by using the sample transferring rod (8), opening the valve I (4) and the valve II (5), and opening the vacuum pump (16) to vacuumize the device;
closing the pneumatic valve (9), closing the valve I (4), opening the helium micro-leakage device (1), enabling helium to enter the test cavity (15) after passing through the gate valve (6) at a constant leakage rate, and starting the mass spectrum (14) to start a calibration process;
thirdly, after the system is stable, a relation curve between the vacuum degree and the helium leakage rate and a relation curve between the helium partial pressure and the helium leakage rate are obtained;
measuring the helium partial pressure of the high-pressure area (10) and the helium partial pressure of the test area (13), estimating effusion according to the known helium partial pressure under the condition of a certain leak rate, and recording the ion current of the mass spectrum (14) to obtain a relation curve of the ion current of the mass spectrum and the effusion;
fifthly, calculating the collision rate of helium atoms with the surface of unit area in unit timeI.e. the number of collisions per unit area per unit time, where p is the gas pressure, m is the molecular mass, k is the Boltzmann constant, T is the temperature, the shutter valve (6) is the shutterThe open area is obtained by the effusion ratio obtained in the step four and the collision rate;
the helium micro-leakage device (1) is closed, the valve II (5) is closed, the sample holder (12) is taken to the test cavity (15) by the sample conveying rod (8), the test cavity (15) is separated into the high-pressure area (10) and the test area (13), the gas storage tank (2) is opened, the valve I (4) is opened, the methane is subjected to a transmittance test, the ion current obtained by the mass spectrum (14) is compared with the relation curve of the ion current of the mass spectrum obtained by the step four and the effusion of helium, and the partial pressure of the methane in the high-pressure area (10) and the test area (13) which are obtained through measurement is calibrated;
seventh calculating the leakage rate of methane from the high pressure zone (10) to the test zone (13) at the sampleWherein A is the open area of the baffle plate of the gate valve (6) obtained in the fifth step, P 1 And P 2 The partial pressure of methane in the high-pressure area (10) and the test area (13) after calibration obtained in the step six, d is the thickness of the sample (11), and Q is the permeability coefficient of methane in the sample material;
and eighthly, multiplying the leak rate of the methane at the sample obtained in the step seven by the partial pressure of the methane in the test area (13) to obtain the transmittance of the methane in the sample (11).
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| CN201710589542.0A CN107389498B (en) | 2017-07-07 | 2017-07-07 | Method for measuring methane transmittance |
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| CN201710589542.0A CN107389498B (en) | 2017-07-07 | 2017-07-07 | Method for measuring methane transmittance |
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