CN117309672A - Integrated module for precisely controlling gas adsorption and desorption by pulsation and control method - Google Patents
Integrated module for precisely controlling gas adsorption and desorption by pulsation and control method Download PDFInfo
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- CN117309672A CN117309672A CN202311598649.3A CN202311598649A CN117309672A CN 117309672 A CN117309672 A CN 117309672A CN 202311598649 A CN202311598649 A CN 202311598649A CN 117309672 A CN117309672 A CN 117309672A
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- 238000001179 sorption measurement Methods 0.000 title claims abstract description 92
- 238000003795 desorption Methods 0.000 title claims abstract description 72
- 238000000034 method Methods 0.000 title claims abstract description 47
- 230000010349 pulsation Effects 0.000 title claims abstract description 37
- 238000007789 sealing Methods 0.000 claims abstract description 622
- 238000000605 extraction Methods 0.000 claims abstract description 387
- 230000008569 process Effects 0.000 claims abstract description 21
- 239000011148 porous material Substances 0.000 claims description 207
- 239000007789 gas Substances 0.000 claims description 89
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 88
- 229910052786 argon Inorganic materials 0.000 claims description 44
- 239000003463 adsorbent Substances 0.000 claims description 37
- 238000005086 pumping Methods 0.000 claims description 32
- 239000002156 adsorbate Substances 0.000 claims description 27
- 230000001105 regulatory effect Effects 0.000 claims description 24
- 238000005259 measurement Methods 0.000 claims description 17
- 238000004140 cleaning Methods 0.000 claims description 11
- 230000001276 controlling effect Effects 0.000 claims description 11
- 238000009530 blood pressure measurement Methods 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 238000012544 monitoring process Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 abstract 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 52
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 39
- 229910052757 nitrogen Inorganic materials 0.000 description 26
- 229910052799 carbon Inorganic materials 0.000 description 9
- 238000004891 communication Methods 0.000 description 7
- 230000008859 change Effects 0.000 description 5
- 238000005273 aeration Methods 0.000 description 4
- 238000005520 cutting process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000012856 packing Methods 0.000 description 3
- 230000035699 permeability Effects 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008094 contradictory effect Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 230000003204 osmotic effect Effects 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
- 238000005406 washing Methods 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
- G01N7/00—Analysing materials by measuring the pressure or volume of a gas or vapour
- G01N7/02—Analysing materials by measuring the pressure or volume of a gas or vapour by absorption, adsorption, or combustion of components and measurement of the change in pressure or volume of the remainder
- G01N7/04—Analysing materials by measuring the pressure or volume of a gas or vapour by absorption, adsorption, or combustion of components and measurement of the change in pressure or volume of the remainder by absorption or adsorption alone
-
- 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
- G01N7/14—Analysing materials by measuring the pressure or volume of a gas or vapour by allowing the material to emit a gas or vapour, e.g. water vapour, and measuring a pressure or volume difference
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- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Combustion & Propulsion (AREA)
- Engineering & Computer Science (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention provides an integrated module for precisely controlling gas adsorption and desorption by pulsation and a control method, and belongs to the technical field of gas adsorption measurement. The integrated module comprises a main body module, a sample tube module, a pressure measuring module, an air path sealing module and a valve module, wherein the pressure measuring module is arranged on the upper portion of the main body module, the sample tube module is arranged on the lower portion of the main body module, the air leakage point of the integrated module is reduced, and the air leakage rate is reduced through end face sealing and radial sealing. Aiming at the condition of a large pressure difference air source, controlling the air inlet adsorption process by adopting a pulse constant volume and filtration permeation mode; and controlling the air extraction and desorption process by a low-resistance straight-through and pulse constant volume mode. The invention solves the problem that the air inlet speed is too high and the adsorption and desorption capacity cannot be controlled in a stepped fixed point mode due to too high pressure difference in the gas adsorption and desorption process.
Description
Technical Field
The invention relates to the technical field of gas adsorption measurement, in particular to an integrated module and a control method for precisely controlling gas adsorption and desorption by pulsation.
Background
When parameters such as specific surface area, pore volume, pore diameter distribution, porosity and the like of the material are measured, the closed small cavity is required to be inflated and pumped, so that the pressure value in the closed small cavity reaches a preset value. At present, the existing measuring device generally adopts methods of installing a flowmeter, adding a buffer cavity, embedding a permeable sheet and the like to reduce the speed of inflation and air extraction, delay the time of pressure change and facilitate accurate control of pressure change; in addition, various components in the device are generally connected by screw threads, so that gas in a closed small cavity leaks under a large pressure difference, and the conservation of gas mass before and after measurement is difficult to ensure; in addition, the device needs to measure the gas adsorption quantity corresponding to different inflation and extraction pressures, the pressure change is in stepwise increasing or decreasing, the adsorption quantity difference corresponding to each step pressure needs to be accurately measured, and the gas quantity charged or extracted each time is required to be smaller than 0.1 mL. The main problems of this type of device are as follows:
(1) The pressure in the closed small cavity is balanced instantaneously under a large pressure difference.
At present, the gas quantity filled into or pumped out of the closed small cavity is controlled by mainly opening or closing or adjusting the valve, and because the closed small cavity is small in space and high in gas flow speed under large pressure difference, the pressure in the closed small cavity is balanced instantaneously, the time required from entering the closed small cavity to pressure balancing is less than the sensing time of the pressure sensor, the executor is difficult to control the gas quantity in time through feedback, and the purpose of controlling the pressure value in the closed small cavity cannot be achieved. In the current adopted solution, the buffer cavity is additionally arranged to delay the problem of too fast air inlet rate, but only the buffer cavity can be inflated according to the size of the buffer cavity, so that the buffer cavity is difficult to accurately control to a preset pressure value; the flowmeter is suitable for an open space, and has no feedback response time to a small closed cavity; the addition of the permeable sheet can effectively reduce the air inlet rate, but the rate of the air passing through the permeable sheet is related to the pressure difference, the pressure difference is high, the pressure difference is low, the permeable sheet is only suitable for the condition of high pressure difference, for the condition of low pressure difference, the time of air charging and air exhausting is prolonged, the leakage amount of the air in the closed space is increased, and the measurement error is increased.
(2) The stepped intake air amount at different differential pressures cannot be controlled accurately.
In the measuring process, the real-time pressure is required to be read at different pressure positions, and the buffer cavity is additionally arranged to replace a continuous flow mode in an intermittent mode, so that the step pressure control can be realized, but because the volume of the buffer cavity is a fixed value, the accurate control of the pressure corresponding to the volume lower than the buffer cavity cannot be realized; the permeation sheet continuously permeates gas under high pressure difference, the permeation rate is reduced along with the reduction of the pressure difference, the permeation rate is high under high pressure difference due to small gas viscosity, the pressure sensor reads the existing time delay, the actual pressure in the small sealing cavity exceeds the preset value when the measured value of the pressure sensor reaches the preset pressure, and the pressure measurement is inaccurate; the pulse valve is additionally arranged to accurately control the pressure change, and because the volume of the expansion hole in the middle of the pulse valve is smaller than the volume corresponding to the preset pressure, the accurate stepped pressure change can be realized under different pressure differences, but when the pressure difference between the inside and the outside of the pulse valve is large, the rebound gasket in the pulse valve cannot be normally opened and closed to stop working due to overlarge pressure, and the pulse valve is disabled under the condition of high pressure difference. Thus, there is a contradictory problem that the osmotic tablet cannot operate under low differential pressure conditions and the pulse valve cannot operate under high differential pressure conditions.
(3) The gas tightness is poor.
The use of the small closed space cavity requires accurate control of the pressure in the small closed space cavity, and strict requirements are put on the tightness of the air passage. The cavity spaces for sealing and measuring the gas in the existing device are all in threaded connection, and when the pressure in the small cavity is too high with the pressure difference of the environment, the air leakage of the connecting part of the pipeline is increased; meanwhile, the threaded connection forms a large amount of dead space at the connection, namely the space for measuring the volume of the material is relatively small, so that the error is increased.
Disclosure of Invention
The invention provides an integrated module and a control method for precisely controlling gas adsorption and desorption by pulsation, which are used for solving the problems that pressure in a closed small cavity is instantaneously balanced under a large pressure difference in a gas adsorption and desorption measurement process, pressure in a sealed small cavity cannot be precisely stepped, air inlet and air exhaust are realized, and air leakage exists due to the fact that a cavity space for sealing measurement gas adopts threaded connection.
In order to achieve the above purpose, the technical scheme provided by the invention is as follows:
the integrated module comprises a main body module, a sample tube module, a pressure measurement module, a gas circuit sealing module and a valve module, wherein the pressure measurement module is arranged on the upper surface of the main body module, the sample tube module is arranged on the lower surface of the main body module, the gas circuit sealing module ensures the sealing of the whole integrated module, and the valve module is arranged on the upper surface and the front surface of the main body module;
The main body module is cuboid, and an air exhaust pipeline interface is arranged on the left side surface of the main body module and used for being connected with a vacuum pump regulating valve; an external air source air inlet hole is formed in the right side surface of the main body module and is used for being connected with an external air source clamping sleeve connector, and a reference cavity cover plate placing groove is formed in the lower portion of the external air source air inlet hole and is used for placing a reference cavity cover plate; the middle part of the upper surface of the main body module is provided with an air pressure sensor sealing ring placing groove for connecting an air pressure sensor, the left side of the air pressure sensor sealing ring placing groove is provided with an air suction three-way valve straight-through air outlet hole, an air suction three-way valve pulsation air outlet hole and an air suction three-way valve air inlet hole for correspondingly accessing the air suction three-way valve, the right side of the air pressure sensor sealing ring placing groove is provided with a sample tube sealing valve air outlet hole and a sample tube sealing valve air inlet hole for correspondingly accessing the sample tube sealing valve, and the right side of the sample tube sealing valve air outlet hole and the sample tube sealing valve air inlet hole is provided with an air charging sealing valve air outlet hole and an air charging sealing valve air inlet hole for correspondingly accessing the air charging sealing valve; the lower surface of the main body module is provided with a sample tube interface mounting groove for mounting the sample tube module; the left side of the front surface of the main body module is provided with an air outlet hole of the air extraction quantitative pulse valve and an air inlet hole of the air extraction quantitative pulse valve, which are used for being correspondingly connected with the air extraction quantitative pulse valve, and the right side of the front surface of the main body module is provided with an air outlet hole of the air inflation quantitative pulse valve and an air inlet hole of the air inflation quantitative pulse valve, which are used for being correspondingly connected with the air inflation quantitative pulse valve.
The air exhaust pipeline connector is provided with a vacuum pump air exhaust coarse pore canal and a vacuum pump air exhaust fine pore canal horizontally and concentrically in the main body module in sequence, the external air source air inlet hole is provided with an external air source air inlet coarse pore canal and an external air source air inlet fine pore canal horizontally and concentrically in the main body module in sequence, the center of the reference cavity cover plate placing groove is provided with a reference cavity sealing ring placing groove and a concentric reference cavity main pore canal opening with the diameter smaller than that of the reference cavity sealing ring placing groove, and the reference cavity main pore canal opening is provided with a reference cavity main pore canal horizontally in the main body module;
the through air outlet of the air suction three-way valve is vertically and downwards provided with an air suction three-way valve through air outlet channel which is communicated with the vacuum pump air suction fine channel; the air pumping three-way valve pulsation air outlet hole is vertically and downwards provided with an air pumping three-way valve pulsation air outlet hole, and the air pumping three-way valve pulsation air outlet hole is communicated with the air pumping quantitative pulse valve air inlet hole; an air inlet channel of the air extraction three-way valve is vertically and downwards opened and communicated with a main channel of the reference cavity;
the air pressure sensor seal ring placing groove is vertically and downwards provided with an air pressure sensor core seat with the concentric diameter smaller than that of the air pressure sensor seal ring placing groove, the air pressure sensor core seat is vertically and downwards provided with an air pressure sensor pore canal, and the air pressure sensor pore canal and the reference cavity main pore canal are intersected at an air pressure sensor pore canal communicating port;
The air outlet hole of the sample tube sealing valve is vertically and downwards provided with a sample tube sealing valve air outlet channel communicated with the sample tube connecting channel, and the air inlet hole of the sample tube sealing valve is vertically and downwards provided with a sample tube sealing valve air inlet channel communicated with the main channel of the reference cavity;
the air outlet hole of the air charging sealing valve is vertically and downwards provided with an air outlet hole channel of the air charging sealing valve which is communicated with the main hole channel of the reference cavity, and the air inlet hole of the air charging sealing valve is vertically and downwards provided with an air inlet hole channel of the air charging sealing valve which is communicated with an air inlet fine hole channel of an external air source;
the air outlet hole of the air charging quantitative pulse valve is horizontally and backwards provided with an air charging quantitative pulse valve air outlet channel communicated with an external air source air inlet thin channel, a non-through air charging quantitative pulse valve expansion hole (the depth of the air charging quantitative pulse valve expansion hole is not more than 1/10 of the front and rear thickness of the main body module) is horizontally and backwards arranged between the air charging quantitative pulse valve air outlet hole and the air charging quantitative pulse valve air inlet hole, and the air charging quantitative pulse valve air inlet channel is horizontally and backwards arranged and communicated with an external air source air inlet thick channel;
the air outlet hole of the air extraction quantitative pulse valve is horizontally and backwards provided with an air outlet hole channel of the air extraction quantitative pulse valve, which is communicated with the air extraction fine hole channel of the vacuum pump, the air outlet hole of the air extraction quantitative pulse valve and the air inlet hole of the air extraction quantitative pulse valve are horizontally and backwards provided with a non-through air extraction quantitative pulse valve expansion hole (the depth of the air extraction quantitative pulse valve expansion hole is not more than 1/10 of the front and rear thickness of the main body module), and the air inlet hole of the air extraction quantitative pulse valve is horizontally and backwards provided with an air inlet hole channel of the air extraction quantitative pulse valve, which is communicated with the air outlet hole channel of the air extraction three-way valve;
The sample tube interface mounting groove is vertically upwards provided with a sample tube interface fixing platform, and the sample tube interface fixing platform is vertically and concentrically upwards provided with a sample tube connecting pore canal.
The air extraction three-way valve is directly connected with the air outlet hole, the air extraction three-way valve pulsation air outlet hole and the air extraction three-way valve air inlet hole, and the two sides of the whole body formed by the air extraction three-way valve pulsation air outlet hole and the air extraction three-way valve air inlet hole are symmetrically provided with an air extraction three-way valve fixing threaded hole and an air extraction three-way valve positioning pin hole, the air extraction three-way valve is positioned on the upper surface of the main body module through the air extraction three-way valve positioning pin hole, forms a seal with the upper surface of the main body module through the air extraction three-way valve sealing ring, and is fixed on the upper surface of the main body module through the air extraction three-way valve fixing threaded hole;
the sample tube sealing valve is positioned on the upper surface of the main body module through the sample tube sealing valve positioning pin hole, forms a seal with the upper surface of the main body module through a sealing valve sealing gasket, and is fixed on the upper surface of the main body module through the sample tube sealing valve fixing threaded hole;
the air inlet and the air outlet of the air sealing valve are symmetrically provided with an air sealing valve fixing threaded hole and an air sealing valve positioning pin hole on two sides of the whole body formed by the air outlet of the air sealing valve and the air inlet of the air sealing valve, the air sealing valve is positioned on the upper surface of the main body module through the air sealing valve positioning pin hole, forms a seal with the upper surface of the main body module through the air sealing valve sealing gasket, and is fixed on the upper surface of the main body module through the air sealing valve fixing threaded hole;
The air outlet hole of the air charging quantitative pulse valve and the air inlet hole of the air charging quantitative pulse valve are symmetrically provided with an air charging quantitative pulse valve fixing threaded hole and an air charging quantitative pulse valve positioning pin hole on both sides of the whole body, the air charging quantitative pulse valve is positioned on the front surface of the main body module through the air charging quantitative pulse valve positioning pin hole, forms a seal with the front surface of the main body module through the air charging quantitative pulse valve sealing gasket, and is fixed on the front surface of the main body module through the air charging quantitative pulse valve fixing threaded hole;
the air outlet hole of the air extraction quantitative pulse valve and the air inlet hole of the air extraction quantitative pulse valve are symmetrically provided with an air extraction quantitative pulse valve fixing threaded hole and an air extraction quantitative pulse valve positioning pin hole on two sides of the whole body, the air extraction quantitative pulse valve is positioned on the front surface of the main body module through an air extraction quantitative pulse valve positioning pin, forms a seal with the front surface of the main body module through an air extraction quantitative pulse valve sealing gasket, and is fixed on the front surface of the main body module through the air extraction quantitative pulse valve fixing threaded hole;
sample tube fixing threaded holes are symmetrically formed in the periphery of the sample tube interface mounting groove, and the sample tube module is fixed to the lower surface of the main body module through the sample tube fixing threaded holes.
The sample tube module comprises a sample tube, a sample tube lock nut combined sealing ring, a sample tube lock nut O-shaped ring, a sample tube interface and a sample tube interface O-shaped ring,
The sample tube locking nut is provided with a sample tube locking nut center hole in the center, the upper surface of the sample tube locking nut is provided with a sample tube locking nut platform, a sample tube locking nut combined sealing ring and a sample tube locking nut O-shaped ring are placed on the sample tube locking nut platform from bottom to top and are installed inside a sample tube connector, the center of the sample tube connector is provided with a sample tube connector center hole, the surface of the sample tube connector is symmetrically provided with a sample tube connector through hole, the center of the upper surface of the sample tube connector is provided with a sample tube connector O-shaped ring placing groove, the sample tube connector O-shaped ring placing groove is internally provided with a sample tube connector O-shaped ring, the sample tube connector is fixed on the lower surface of the main body module through a sample tube fixing threaded hole and the sample tube connector through the sample tube locking nut, the sample tube locking nut combined sealing ring and the sample tube locking nut O-shaped ring, and the sample tube locking nut O-shaped ring are fastened through threads, so that the sample tube locking nut O-shaped ring is fastened to expand and compress the sample tube in the radial direction;
the enclosed volume surrounded by the air outlet hole of the sample tube sealing valve, the connecting pore canal of the sample tube, the air outlet pore canal of the sample tube sealing valve and the sample tube on the main body module is called a sample cavity;
The enclosed volume surrounded by the air suction three-way valve air inlet, the air pressure sensor sealing ring placing groove, the sample tube sealing valve air inlet, the air inflation sealing valve air outlet and the reference cavity cover plate is called a reference cavity.
The gas path sealing module comprises a vacuum pump regulating valve, a vacuum pump assembling sealing ring, an external gas source clamping sleeve joint, an external gas source assembling sealing ring, a reference cavity sealing O-shaped ring and a reference cavity cover plate,
the reference cavity sealing O-shaped ring is arranged in the reference cavity sealing ring placing groove, an end face seal is formed by compressing the reference cavity cover plate, an inflatable filter is arranged at the joint of the external air source air inlet coarse pore canal and the external air source air inlet fine pore canal, an external air source clamping sleeve joint is fixed on the right side surface of the main body module through threads in an external air source air inlet hole, the external air source combined sealing ring is compressed to form a seal, and the inflatable filter is compressed through the external air source combined sealing ring;
the vacuum pump regulating valve is fixed on the left side surface of the main body module through threads in the air extraction pipeline interface, and compresses the vacuum pump combined sealing ring to form a seal;
four reference cavity cover plate through holes are symmetrically formed in the periphery of the reference cavity cover plate, reference cavity cover plate fixing threaded holes are symmetrically formed in the periphery of the reference cavity cover plate placing groove, fastening screws are screwed into the reference cavity cover plate fixing threaded holes through the four reference cavity cover plate through holes to be fixed on the right side surface of the main body module, and reference cavity sealing O-shaped rings are placed in the reference cavity sealing ring placing groove.
The valve module comprises an air extraction three-way valve, an air extraction three-way valve sealing ring, a sample tube sealing valve sealing gasket, an air inflation sealing valve sealing gasket, an air inflation quantitative pulse valve sealing gasket, an air extraction quantitative pulse valve and an air extraction quantitative pulse valve sealing gasket, wherein the valves of the valve module are seat-mounted electromagnetic valves and are sealed with a smooth plane through the sealing gaskets;
the lower surface of the air extraction three-way valve is horizontally provided with an air extraction three-way valve fixing through hole, an air extraction three-way valve through air outlet, an air extraction three-way valve pulsation air outlet, an air extraction three-way valve air inlet and an air extraction three-way valve positioning pin, the lower surface of the air extraction three-way valve is provided with an air extraction three-way valve sealing groove, and an air extraction three-way valve sealing gasket is placed in the air extraction three-way valve sealing groove; when the air extraction three-way valve is in a closed state, the air inlet of the air extraction three-way valve is communicated with the through air outlet of the air extraction three-way valve, and the air inlet of the air extraction three-way valve is blocked with the pulsating air outlet of the air extraction three-way valve; when the air extraction three-way valve is in an open state, the air inlet of the air extraction three-way valve is blocked from the through air outlet of the air extraction three-way valve, and the air inlet of the air extraction three-way valve is communicated with the pulsating air outlet of the air extraction three-way valve;
The lower surface center of the air extraction quantitative pulse valve is symmetrically provided with an air extraction quantitative pulse valve fixing through hole and an air extraction quantitative pulse valve positioning pin, the center of the lower surface of the air extraction quantitative pulse valve is provided with an air extraction quantitative pulse valve expansion port, two sides of the air extraction quantitative pulse valve expansion port are symmetrically provided with an air extraction quantitative pulse valve air inlet and an air extraction quantitative pulse valve air outlet, the lower surface of the air extraction quantitative pulse valve is provided with an air extraction quantitative pulse valve sealing groove, and an air extraction quantitative pulse valve sealing gasket is placed in the air extraction quantitative pulse valve sealing groove; when the air extraction quantitative pulse valve is in an open state, the air inlet of the air extraction quantitative pulse valve and the air outlet of the air extraction quantitative pulse valve are alternately opened and closed at the frequency of 10Hz, the air between the air inlet of the air extraction quantitative pulse valve and the air outlet of the air extraction quantitative pulse valve is discharged, and when the air extraction quantitative pulse valve is in a closed state, the air inlet of the air extraction quantitative pulse valve is kept sealed to block the air;
the center of the lower surface of the sample tube sealing valve is symmetrically provided with a sample tube sealing valve fixing through hole and a sample tube sealing valve positioning pin, the center of the lower surface of the sample tube sealing valve is provided with a sample tube sealing valve air inlet, the side of the sample tube sealing valve air inlet is provided with a sample tube sealing valve air outlet, the lower surface of the sample tube sealing valve is provided with a sample tube sealing valve sealing groove, and a sample tube sealing gasket is placed in the sample tube sealing valve sealing groove; when the sample tube sealing valve is in an open state, an air inlet of the sample tube sealing valve is communicated with an air outlet of the sample tube sealing valve; when the sample tube sealing valve is in a closed state, the air inlet of the sample tube sealing valve is blocked from the air outlet of the sample tube sealing valve;
The center of the lower surface of the quantitative inflation pulse valve is symmetrically provided with two quantitative inflation pulse valve fixing through holes and quantitative inflation pulse valve positioning pins, the center of the lower surface of the quantitative inflation pulse valve is provided with quantitative inflation pulse valve expansion openings, two sides of each quantitative inflation pulse valve expansion opening are symmetrically provided with quantitative inflation pulse valve air outlets and quantitative inflation pulse valve air inlets, and are provided with quantitative inflation pulse valve sealing grooves, and quantitative inflation pulse valve sealing gaskets are placed in the quantitative inflation pulse valve sealing grooves; when the quantitative inflation pulse valve is in an open state, the air inlet of the quantitative inflation pulse valve and the air outlet of the quantitative inflation pulse valve are alternately opened and closed at the frequency of 10Hz, and the air between the air inlet of the quantitative inflation pulse valve and the air outlet of the quantitative inflation pulse valve is discharged; when the quantitative inflation pulse valve is in a closed state, the air inlet of the quantitative inflation pulse valve is kept sealed to block the air;
the center of the lower surface of the inflatable sealing valve is symmetrically provided with two inflatable sealing valve fixing through holes and an inflatable sealing valve positioning pin, the center of the lower surface of the inflatable sealing valve is provided with an inflatable sealing valve air outlet, the side of the inflatable sealing valve air outlet is provided with an inflatable sealing valve air inlet, the lower surface of the inflatable sealing valve is provided with an inflatable sealing valve sealing groove, and an inflatable sealing valve sealing gasket is placed in the inflatable sealing valve sealing groove; when the air charging sealing valve is in an open state, an air inlet of the air charging sealing valve is communicated with an air outlet of the air charging sealing valve; when the air charging sealing valve is in a closed state, the air inlet of the air charging sealing valve is blocked from the air outlet of the air charging sealing valve.
The three-way valve positioning pin on the three-way valve aligns with the three-way valve positioning pin hole on the main body module, the through air outlet of the three-way valve on the three-way valve is communicated with the through air outlet of the three-way valve on the main body module, the pulsating air outlet of the three-way valve on the three-way valve is communicated with the pulsating air outlet of the three-way valve on the main body module, the air inlet of the three-way valve on the three-way valve is communicated with the air inlet hole of the three-way valve on the main body module, the fastening screw is screwed into the three-way valve fixing threaded hole on the main body module through the three-way valve fixing through hole on the three-way valve, and after the fastening screw is screwed, the three-way valve forms a seal with the main body module;
the air inlet of the air quantitative pulse valve on the air quantitative pulse valve is communicated with the air inlet of the air quantitative pulse valve on the main body module, the fastening screw is screwed into the air quantitative pulse valve fixing threaded hole on the main body module through the air quantitative pulse valve fixing through hole on the air quantitative pulse valve, and after the fastening screw is screwed up, the air quantitative pulse valve and the main body module form a seal;
The air suction quantitative pulse valve positioning pin on the air suction quantitative pulse valve is aligned with the air suction quantitative pulse valve positioning pin hole on the main body module, the air suction quantitative pulse valve air inlet on the air suction quantitative pulse valve is communicated with the air suction quantitative pulse valve air inlet on the main body module, the air suction quantitative pulse valve expansion port on the air suction quantitative pulse valve is communicated with the air suction quantitative pulse valve expansion hole on the main body module, the air outlet of the air suction quantitative pulse valve on the air suction quantitative pulse valve is communicated with the air outlet of the air suction quantitative pulse valve on the main body module, the fastening screw is screwed into the air suction quantitative pulse valve fixing threaded hole on the main body module through the air suction quantitative pulse valve fixing through hole on the air suction quantitative pulse valve, and after the fastening screw is screwed up, the air suction quantitative pulse valve and the main body module form a seal;
the sample tube sealing valve positioning pin on the sample tube sealing valve is aligned with the sample tube sealing valve positioning pin hole on the main body module, the sample tube sealing valve air inlet on the sample tube sealing valve is communicated with the sample tube sealing valve air inlet on the main body module, the sample tube sealing valve air outlet on the sample tube sealing valve is communicated with the sample tube sealing valve air outlet on the main body module, the fastening screw is screwed into the sample tube sealing valve fixing threaded hole on the main body module through the sample tube sealing valve fixing through hole on the sample tube sealing valve, and after the fastening screw is screwed, the sample tube sealing valve and the main body module form sealing;
The air-filled sealing valve positioning pin on the air-filled sealing valve is aligned with the air-filled sealing valve positioning pin hole on the main body module, the air inlet of the air-filled sealing valve on the air-filled sealing valve is communicated with the air inlet of the air-filled sealing valve on the main body module, the air outlet of the air-filled sealing valve on the air-filled sealing valve is communicated with the air outlet of the air-filled sealing valve on the main body module, the fastening screw is screwed into the air-filled sealing valve fixing threaded hole on the main body module through the air-filled sealing valve fixing through hole on the air-filled sealing valve, and after the fastening screw is screwed, the air-filled sealing valve and the main body module form sealing.
The invention also provides a control method of the integrated module for controlling the adsorption and desorption of the gas by pulsation, which comprises the following steps:
s1, filling an adsorbent: unscrewing a sample tube locking nut, taking down the sample tube, weighing the mass of the sample tube, loading the adsorbent to be tested, weighing the total mass of the sample tube and the adsorbent, inserting the sample tube into a sample tube interface, screwing the sample tube locking nut to finish the filling of the adsorbent, placing the sample tube containing the adsorbent into a liquid adsorbent, and closing all valves;
s2, cleaning the reference cavity and the sample cavity: switching an external air source to high-purity argon, opening an external vacuum pump, adjusting a vacuum pump adjusting valve, closing an air extraction three-way valve, switching to an air flow straight-through state, vacuumizing a reference cavity, opening a sample tube sealing valve to vacuumize the sample cavity after 10 seconds, switching the air extraction three-way valve to an air flow closing state to stop air extraction when the pressure reaches below 0.001 Pa after the reference cavity and the gas in the sample cavity pass through a sample tube connecting pore channel, a sample tube sealing valve air outlet pore channel, a sample tube sealing valve air inlet pore channel, a reference cavity main pore channel, an air extraction three-way valve air inlet pore channel, an air extraction three-way valve straight-through air outlet pore channel, a vacuum pump air exhaust fine pore channel, a vacuum pump air exhaust coarse pore channel and a vacuum pump adjusting valve are arranged, opening an inflation sealing valve, filling argon into a reference cavity and a sample cavity, enabling the argon to enter a main body module through an external air source clamping sleeve joint, enabling the argon to enter an external air source air inlet thin pore channel through an external air source air inlet thick pore channel and an inflation filter piece, enabling an inflation sealing valve air inlet pore channel and an inflation sealing valve air outlet pore channel to enter a reference cavity main pore channel, enabling part of the argon in the reference cavity main pore channel to enter a core seat of a pneumatic sensor, enabling the other part of the argon to enter a sample tube sealing valve air inlet pore channel, a sample tube sealing valve and a sample tube sealing valve air outlet pore channel, enabling the argon to enter a sample tube through a sample tube connecting pore channel, closing the inflation sealing valve when the pressure value measured by the pneumatic sensor reaches 27-30 kPa, and closing the sample tube sealing valve after 10 seconds, so as to finish one-time cleaning;
S3, air volume calibration: repeating the step S2 four times to finish the replacement cleaning of the reference cavity and the sample cavity; switching the air suction three-way valve to an air flow through state, vacuumizing the reference cavity, opening the sample tube sealing valve to vacuumize the sample cavity after 10 seconds, measuring and recording the pressure at the moment by the air pressure sensor after 10 seconds when the pressure reaches below 0.001 Pa, opening the air suction three-way valve to an air flow closing state, measuring and recording the pressure at the moment by the air pressure sensor, opening an inflatable sealing valve to charge argon into a reference cavity, enabling the argon to enter a main body module through an external air source clamping sleeve joint, enabling an external air source air inlet rough pore channel, an inflatable filter piece, an external air source air inlet fine pore channel, an inflatable sealing valve air inlet pore channel, an inflatable sealing valve and an inflatable sealing valve air outlet pore channel to enter a reference cavity main pore channel, enabling part of the argon in the reference cavity main pore channel to enter a pressure sensor core seat, enabling the other part of the argon to enter a sample tube sealing valve air inlet pore channel, closing the inflatable sealing valve when the pressure sensor detects that the pressure is 27-30 kPa, measuring and recording the pressure value at the moment after 10 seconds, opening the sample tube sealing valve, enabling the argon to enter a sample tube through the sample tube sealing valve, the sample tube sealing valve air outlet pore channel and the sample tube connecting pore channel, and monitoring the gas pressure in real time by the pressure sensor, and measuring and recording the pressure value at the moment after 10 seconds;
S4, measuring adsorption data points at low pressure: closing a sample tube sealing valve, starting a vacuum pump, closing an air extraction three-way valve, switching to an air flow through state, vacuumizing a reference cavity, opening the sample tube sealing valve after 10 seconds, vacuumizing the sample cavity, enabling argon in the reference cavity and the sample cavity to directly pass through an air inlet channel of the air extraction three-way valve, an air outlet channel of the air extraction three-way valve, an air pumping fine channel of the vacuum pump, a coarse channel of the vacuum pump and a regulating valve of the vacuum pump, measuring gas pressure by a pressure sensor, opening the air extraction three-way valve to a gas flow closing state when the pressure reaches below 0.001 Pa, measuring the pressure at the moment after 10 seconds, closing the sample tube sealing valve, connecting an external air source clamping sleeve joint with a high-purity adsorbate gas cylinder, opening the air filling sealing valve into the reference cavity, enabling adsorbate to enter a main module through the external air source clamping sleeve joint, enabling the external air inlet coarse channel, the air inlet fine channel of the air source, the air inlet sealing valve and the air inlet fine channel of the air filling sealing valve to enter the main channel of the reference cavity, enabling part of the adsorbate to enter a core seat of the air pressure sensor when the pressure of the pressure sensor to be divided into two flow directions, and when the pressure of the adsorption mass enters the core seat of the air pressure sensor is measured, and the pressure of the pressure sensor is measured after 10 seconds, and the pressure of the sample tube is measured after 10 seconds is recorded, and the pressure is measured;
S5, measuring adsorption data points at high pressure: when the pressure sensor monitors that the pressure in the main pore canal of the reference cavity is higher than 25 kPa, the time required for air intake of the air-filled filter piece is increased, so that the air leakage of the sample cavity and the reference cavity is increased, at the moment, the air intake of the air-filled quantitative pulse valve is switched to, the adsorbate enters the main module through an external air source clamping sleeve joint, and enters the main module through an external air source air intake rough pore canal, an air-filled quantitative pulse valve air intake pore canal, an air-filled quantitative pulse valve air outlet pore canal, an external air source air intake fine pore canal, an air-filled sealing valve air intake pore canal, an air-filled sealing valve air-outlet pore canal and an air-filled sealing valve air-outlet pore canal enter the main pore canal of the reference cavity, wherein the adsorbate in the main pore canal of the reference cavity is divided into two flow directions, one part of adsorbate enters the air-pressure sensor core seat, the other part of adsorbate enters the air-inlet pore canal of the sample tube sealing valve, the air-filled sealing valve is closed, the air pressure value is measured and recorded after 10 seconds, the sample tube sealing valve is opened, and the air pressure value is measured and recorded at the moment after 10 seconds;
s6, repeating the step S5 until the air pressure sensor detects that the pressure in the reference cavity reaches a standard atmospheric pressure, stopping measuring adsorption data, and drawing an isothermal adsorption line at the temperature according to a measurement result;
S7, determination of desorption data points at high pressure: measuring isothermal desorption lines by taking the state at the end of the adsorption process as an initial state, closing all valves, and placing a sample tube containing the adsorbent in a temperature environment where the adsorbent is still positioned in the adsorption process, wherein the absolute pressure at the interface of an air extraction pipeline is close to 0 kPa; at the moment, the pressure difference at the interface of the pressure in the reference cavity and the air extraction pipeline is too large, the pressure in the reference cavity can be changed too fast through direct air extraction, and the air extraction three-way valve is not fed back timely due to measurement lag of the air pressure sensor, so that the air extraction quantitative pulse valve is adopted for air extraction; switching the air extraction three-way valve to an air flow closing state, opening the air extraction quantitative pulse valve to extract air from the reference cavity, opening the air extraction quantitative pulse valve to extract the air from the reference cavity main pore canal, and measuring and recording the air pressure value at the moment after 10 seconds, opening the sample tube sealing valve, and measuring and recording the pressure value at the moment after 10 seconds;
S8, measuring desorption data points at low pressure: when the balance pressure is lower than the absolute pressure of 25 kPa, the pressure difference between the inside and the outside of the air extraction quantitative pulse valve is too small, the time required for air extraction by using the air extraction quantitative pulse valve is increased, so that the air leakage of the sample cavity and the reference cavity is increased, and at the moment, the air extraction three-way valve is required to be closed to be switched to an air flow through state for air extraction; closing a sample tube sealing valve, switching the air extraction three-way valve to an air flow through state to extract air from a reference cavity, discharging the air in a main pore canal of the reference cavity through an air inlet pore canal of the air extraction three-way valve, a direct air outlet pore canal of the air extraction three-way valve, a vacuum pump air suction fine pore canal, a vacuum pump air suction coarse pore canal and a vacuum pump regulating valve, opening the air extraction three-way valve to an air flow closing state to stop air extraction when the pressure value detected by an air pressure sensor reaches a preset pressure of +/-1 kPa, measuring and recording the pressure after 10 seconds, opening the sample tube sealing valve, and measuring and recording the pressure after 10 seconds;
s9, repeating the steps S7 and S8 until the pressure sensor detects that the pressure reaches below 0.001 and Pa absolute pressure, stopping measuring desorption data, and drawing an isothermal desorption line at the temperature according to the measurement result;
S10, residual gas treatment: and opening the sealing valve of the sample tube, closing the air extraction three-way valve, switching the air extraction three-way valve to an air flow through state, and discharging air in the sample cavity and the reference cavity through the air inlet pore canal of the air extraction three-way valve, the air outlet pore canal of the air extraction three-way valve, the air pumping fine pore canal of the vacuum pump, the air pumping coarse pore canal of the vacuum pump and the regulating valve of the vacuum pump, wherein the air pressure sensor measures the air pressure, and when the pressure is less than 0.001 Pa, opening the air extraction three-way valve, switching the air extraction three-way valve to an air flow closing state, and stopping air extraction.
Compared with the prior art, the technical scheme has at least the following beneficial effects:
the scheme solves the problem that the air inlet speed is too high and the adsorption and desorption capacity cannot be controlled in a stepped fixed point mode due to the fact that the pressure difference is too high in the gas adsorption and desorption process; the problem that the stepped air inflow and the pumping-up amount under different pressure differences in the gas adsorption and desorption processes cannot be accurately controlled is solved; the problem of poor air tightness inside the threaded connection pipeline device is solved.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required for the description of the embodiments will be briefly described below, and it is apparent that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is an exploded view of an integrated module for pulsating accurate control of gas adsorption and desorption in accordance with the present invention;
FIG. 2 is a perspective view 1 of a body module in an integrated module for pulsed accurate control of gas adsorption and desorption in accordance with the present invention;
FIG. 3 is a perspective view 2 of a body module in an integrated module for pulsed accurate control of gas adsorption and desorption in accordance with the present invention;
FIG. 4 is an exploded view of a sample tube module in an integrated module for pulsed accurate control of gas adsorption and desorption in accordance with the present invention;
FIG. 5 is an external view of a pumping quantitative pulse valve in a valve module of an integrated module for pulsating accurate control of gas adsorption and desorption according to the present invention;
FIG. 6 is an external view of an extraction three-way valve in a valve module of an integrated module for pulsating accurate control of gas adsorption and desorption according to the present invention;
FIG. 7 is an external view of a sample tube sealing valve in a valve module of an integrated module for pulsating accurate control of gas adsorption and desorption in accordance with the present invention;
FIG. 8 is an external view of a pneumatic proportional pulse valve in a valve module of an integrated module for pulsating precise control of gas adsorption and desorption in accordance with the present invention;
fig. 9 is an external view of a gas-filled sealing valve in a valve module of an integrated module for pulsating accurate control of gas adsorption and desorption according to the present invention.
Wherein the reference numerals are as follows:
100-a main body module, 101-an air extraction three-way valve fixing threaded hole, 102-an air extraction three-way valve straight-through air outlet hole, 103-an air extraction three-way valve pulsation air outlet hole, 104-an air extraction three-way valve air inlet hole, 105-an air extraction three-way valve positioning pin hole, 106-an air pressure sensor fixing threaded hole, 107-an air pressure sensor sealing ring placing groove, 108-an air pressure sensor core seat, 109-a sample tube sealing valve fixing threaded hole, 110-a sample tube sealing valve air outlet hole, 111-a sample tube sealing valve air inlet hole, 112-a sample tube sealing valve positioning pin hole, 113-an air filling sealing valve fixing threaded hole, 114-an air filling sealing valve air outlet hole, 115-an air filling sealing valve positioning pin hole, 116-an air filling sealing valve air inlet hole and 117-an external air source air inlet fine pore, 118-external air source air inlet rough pore, 119-external air source air inlet hole, 120-inflating quantitative pulse valve air outlet hole, 121-inflating quantitative pulse valve air inlet hole, 122-inflating quantitative pulse valve fixing threaded hole, 123-inflating quantitative pulse valve positioning pin hole, 124-reference cavity cover plate placing groove, 125-reference cavity cover plate fixing threaded hole, 126-reference cavity main pore, 127-sample tube fixing threaded hole, 128-sample tube connecting pore, 129-air extraction quantitative pulse valve fixing threaded hole, 130-air extraction quantitative pulse valve positioning pin hole, 131-air extraction quantitative pulse valve air outlet hole, 132-air extraction three-way valve air inlet pore, 133-air extraction quantitative pulse valve air inlet hole, 134-air extraction quantitative pulse valve air inlet pore, 135-air extraction quantitative pulse valve air outlet pore, 136-vacuum pump air suction fine pore canal, 137-vacuum pump air suction coarse pore canal, 138-air suction pipeline joint, 139-air suction three-way valve pulsation air outlet pore canal, 140-air suction three-way valve through air outlet pore canal, 141-air suction sealing valve air inlet pore canal, 142-air suction quantitative pulse valve expansion pore canal, 143-air suction sealing valve air outlet pore canal, 144-air suction quantitative pulse valve air outlet pore canal, 145-air suction quantitative pulse valve air inlet pore canal, 146-reference cavity sealing ring placing groove, 147-reference cavity main pore canal orifice, 148-sample pipe sealing valve air outlet pore canal, 149-sample pipe joint mounting groove, 150-sample pipe joint fixing platform, 151-sample pipe sealing valve air inlet pore canal, 152-air pressure sensor pore canal communication port, 153-air suction three-way valve air inlet pore canal communication port, 154-air pressure sensor pore canal, 155-air suction quantitative pulse valve air outlet communication port, 156-air suction quantitative pulse valve air inlet pore canal communication port, 157-air suction quantitative pulse valve expansion pore canal, 158-air suction ventilation sheet, 159-external air source combined sealing ring, 160-external air source joint, 161-reference cavity sealing ring, 162-reference cavity sealing cover plate, 163-reference cavity sealing ring, 165-reference cavity cover plate, 165-reference cavity sealing pump cover plate, and 165-vacuum pump joint;
200-sample tube, 201-sample tube lock nut, 202-sample tube lock nut central hole, 203-sample tube lock nut platform, 204-sample tube lock nut combined sealing ring, 205-sample tube lock nut O-shaped ring, 206-sample tube interface, 207-sample tube interface central hole, 208-sample tube interface O-shaped ring placing groove, 209-sample tube interface through hole, 210-sample tube interface O-shaped ring;
301-bleed three-way valve, 302-bleed three-way valve seal ring, 303-sample tube seal valve, 304-sample tube seal valve gasket, 305-gas-filled seal valve, 306-gas-filled seal valve gasket, 307-gas-filled dosing pulse valve gasket, 308-gas-filled dosing pulse valve, 309-bleed dosing pulse valve, 310-bleed dosing pulse valve gasket, 311-bleed dosing pulse valve fixed through-hole, 312-bleed dosing pulse valve air inlet, 313-bleed dosing pulse valve expansion port, 314-bleed dosing pulse valve air outlet, 315-bleed dosing pulse valve sealing groove, 316-bleed dosing pulse valve positioning pin, 317-bleed three-way valve fixed through-hole, 318-bleed three-way valve through-air outlet, 320-bleed three-way valve pulse air outlet, 320-bleed three-way valve air inlet, 321-bleed three-way valve sealing groove, 322-bleed three-way valve positioning pin, 323-sample tube sealing through-hole, 324-sample tube sealing valve positioning pin, 326-sample tube sealing valve air outlet, 327-sample tube sealing groove, 328-gas-filling pulse valve fixed through-hole, 328-gas outlet, dosing pulse valve expansion port, 317-air outlet, 329-dosing pulse valve expansion port, 329-air inlet, dosing pulse valve expansion port, 332-air inlet, and air inlet valve fixed through-fill valve fixed through-hole, 332-air inlet valve air inlet, and air valve fixed through-vent valve air outlet, 338-an inflatable sealing valve sealing the groove;
401-air pressure sensor fastening end plate center hole, 402-air pressure sensor fastening end plate, 403-air pressure sensor fastening end plate through hole, 404-air pressure sensor end face sealing O-shaped ring, 405-air pressure sensor fastening end plate groove, 406-air pressure sensor, 407-air pressure sensor radial sealing O-shaped ring.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more clear, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings of the embodiments of the present invention. It will be apparent that the described embodiments are some, but not all, embodiments of the invention. All other embodiments, which can be made by a person skilled in the art without creative efforts, based on the described embodiments of the present invention fall within the protection scope of the present invention.
It should be noted that "upper", "lower", "left", "right", "front", "rear", and the like are used in the present invention only to indicate a relative positional relationship, and when the absolute position of the object to be described is changed, the relative positional relationship may be changed accordingly.
The invention provides an integrated module for precisely controlling gas adsorption and desorption by pulsation and a control method.
As shown in fig. 1, the integrated module comprises a main body module 100, a sample tube module, a pressure measurement module, a gas path sealing module and a valve module, wherein the pressure measurement module is installed on the upper surface of the main body module 100, the sample tube module is installed on the lower surface of the main body module 100, the gas path sealing module ensures the sealing of the whole integrated module, and the valve module is installed on the upper surface and the front surface of the main body module 100;
the air pressure sensor 406 is fixed on the upper surface of the main body module 100 through the air pressure sensor fastening end plate 402, an air pressure sensor radial sealing O-shaped ring 407 is arranged between the air pressure sensor 406 and the upper surface of the main body module 100, an air pressure sensor end face sealing O-shaped ring 404 is arranged between the air pressure sensor 406 and the air pressure sensor fastening end plate 402, an air pressure sensor fastening end plate groove 405 is formed in the middle of the air pressure sensor 406, an air pressure sensor fastening end plate central hole 401 is formed in the center of the air pressure sensor fastening end plate 402, and air pressure sensor fastening end plate through holes 403 are symmetrically formed in the air pressure sensor fastening end plate 402.
As shown in fig. 2 and 3, wherein fig. 2 is a top view, fig. 3 is a bottom view, the main body module 100 is a cuboid, and an air exhaust pipe interface 138 is formed on the left side surface of the main body module 100 and is used for connecting with a vacuum pump adjusting valve 165; an external air source air inlet hole 119 is formed in the right side surface of the main body module 100 and is used for being connected with an external air source clamping sleeve joint 160, and a reference cavity cover plate placing groove 124 is formed in the lower portion of the external air source air inlet hole 119 and is used for placing a reference cavity cover plate 162; the middle part of the upper surface of the main body module 100 is provided with an air pressure sensor sealing ring placing groove 107, an air pressure sensor 406 is fixed through an air pressure sensor fixing threaded hole 106 around the air pressure sensor sealing ring placing groove 107, the left side of the air pressure sensor sealing ring placing groove 107 is provided with an air suction three-way valve through air outlet hole 102, an air suction three-way valve pulsation air outlet hole 103 and an air suction three-way valve air inlet hole 104 for corresponding access to an air suction three-way valve 301, the right side of the air pressure sensor sealing ring placing groove 107 is provided with a sample tube sealing valve air outlet hole 110 and a sample tube sealing valve air inlet hole 111 for corresponding access to a sample tube sealing valve 303, and the right sides of the sample tube sealing valve air outlet hole 110 and the sample tube sealing valve air inlet hole 111 are provided with an air charging sealing valve air outlet hole 114 and an air charging sealing valve air inlet hole 116 for corresponding access to an air charging sealing valve 305; the lower surface of the main body module 100 is provided with a sample tube interface mounting groove 149 for mounting the sample tube module; the left side of the front surface of the main body module 100 is provided with an air extraction quantitative pulse valve air outlet hole 131 and an air extraction quantitative pulse valve air inlet hole 133 for correspondingly accessing the air extraction quantitative pulse valve 309, and the right side of the front surface of the main body module 100 is provided with an air inflation quantitative pulse valve air outlet hole 120 and an air inflation quantitative pulse valve air inlet hole 121 for correspondingly accessing the air inflation quantitative pulse valve 308.
The air suction pipeline interface 138 is provided with a vacuum pump air suction rough duct 137 and a vacuum pump air suction fine duct 136 with smaller diameters in a horizontal and concentric manner in the main body module 100, the external air source air inlet 119 is provided with an external air source air inlet rough duct 118 and an external air source air inlet fine duct 117 with smaller diameters in a horizontal and concentric manner in the main body module 100, the center of the reference cavity cover plate placing groove 124 is provided with a reference cavity sealing ring placing groove 146 and a reference cavity main duct opening 147 which is concentric and has a diameter smaller than that of the reference cavity sealing ring placing groove 146, and the reference cavity main duct opening 147 is provided with a reference cavity main duct 126 in a horizontal manner in the main body module 100;
the air-extracting three-way valve through air outlet hole 102 is vertically and downwardly provided with an air-extracting three-way valve through air outlet hole 140, and the air-extracting three-way valve through air outlet hole 140 is communicated with the vacuum pump air exhausting fine hole 136; the pumping three-way valve pulsation air outlet hole 103 is vertically and downwards provided with a pumping three-way valve pulsation air outlet hole 139, and the pumping three-way valve pulsation air outlet hole 139 is communicated with the pumping quantitative pulse valve air inlet hole 134 and is communicated with the pumping quantitative pulse valve air inlet hole communication port 156; the air inlet hole 104 of the air extraction three-way valve is vertically and downwards provided with an air inlet hole 132 of the air extraction three-way valve, and the air inlet hole 132 of the air extraction three-way valve is communicated with the main hole 126 of the reference cavity and is communicated with the air inlet hole communicating opening 153 of the air extraction three-way valve;
The air pressure sensor seal ring placing groove 107 is vertically and downwardly provided with an air pressure sensor core seat 108 with a concentric diameter smaller than that of the air pressure sensor seal ring placing groove 107, the air pressure sensor core seat 108 is vertically and downwardly provided with an air pressure sensor pore canal 154, and the air pressure sensor pore canal 154 and the reference cavity main pore canal 126 intersect at an air pressure sensor pore canal communication port 152;
the sample tube sealing valve air outlet hole 110 is vertically and downwardly provided with a sample tube sealing valve air outlet hole 148 communicated with the sample tube connecting hole 128, and the sample tube sealing valve air inlet hole 111 is vertically and downwardly provided with a sample tube sealing valve air inlet hole 151 communicated with the reference cavity main hole 126;
the air outlet hole 114 of the air charging sealing valve is vertically and downwards provided with an air outlet hole 143 of the air charging sealing valve, which is communicated with the main hole 126 of the reference cavity, and the air inlet hole 116 of the air charging sealing valve is vertically and downwards provided with an air inlet hole 141 of the air charging sealing valve, which is communicated with the air inlet fine hole 117 of the external air source;
the air outlet hole 120 of the air charging quantitative pulse valve is horizontally and backwardly provided with an air charging quantitative pulse valve air outlet channel 144 communicated with the air inlet thin channel 117 of the external air source, the air charging quantitative pulse valve air outlet hole 120 and the air charging quantitative pulse valve air inlet hole 121 are horizontally and backwardly provided with a non-through air charging quantitative pulse valve expansion hole 142, and the air charging quantitative pulse valve air inlet hole 121 is horizontally and backwardly provided with an air charging quantitative pulse valve air inlet channel 145 communicated with the air inlet thick channel 118 of the external air source;
The air outlet hole 131 of the air extraction quantitative pulse valve is horizontally and backwardly provided with an air outlet hole 135 of the air extraction quantitative pulse valve, which is communicated with the air outlet hole 136 of the vacuum pump, and is communicated with the air outlet hole communication port 155 of the air extraction quantitative pulse valve, the air outlet hole 131 of the air extraction quantitative pulse valve and the air inlet hole 133 of the air extraction quantitative pulse valve are horizontally and backwardly provided with a non-through air extraction quantitative pulse valve expansion hole 157, and the air inlet hole 133 of the air extraction quantitative pulse valve is horizontally and backwardly provided with an air inlet hole 134 of the air extraction quantitative pulse valve, which is communicated with the air outlet hole 139 of the air extraction three-way valve;
the sample tube interface mounting groove 149 is vertically and upwardly provided with a sample tube interface fixing platform 150, and the sample tube interface fixing platform 150 is vertically and concentrically provided with a sample tube connecting duct 128.
The air extraction three-way valve through air outlet hole 102, air extraction three-way valve pulsation air outlet hole 103 and air extraction three-way valve air inlet hole 104 are formed on two sides of the whole symmetrically, an air extraction three-way valve fixing threaded hole 101 and an air extraction three-way valve positioning pin hole 105 are formed in the whole, an air extraction three-way valve 301 is positioned on the upper surface of the main body module 100 through the air extraction three-way valve positioning pin hole 105, and is sealed with the upper surface of the main body module 100 through an air extraction three-way valve sealing ring 302, and is fixed on the upper surface of the main body module 100 through the air extraction three-way valve fixing threaded hole 101;
The sample tube sealing valve air outlet hole 110 and the sample tube sealing valve air inlet hole 111 are formed in two sides of the whole body symmetrically, a sample tube sealing valve fixing threaded hole 109 and a sample tube sealing valve positioning pin hole 112 are formed in the whole body, a sample tube sealing valve 303 is positioned on the upper surface of the main body module 100 through the sample tube sealing valve positioning pin hole 112, forms sealing with the upper surface of the main body module 100 through a sealing valve sealing gasket 304, and is fixed on the upper surface of the main body module 100 through the sample tube sealing valve fixing threaded hole 109;
the air-filled sealing valve air outlet hole 114 and the air-filled sealing valve air inlet hole 116 are formed in two sides of the whole body symmetrically, and an air-filled sealing valve fixing threaded hole 113 and an air-filled sealing valve positioning pin hole 115 are formed in the whole body, the air-filled sealing valve 305 is positioned on the upper surface of the main body module 100 through the air-filled sealing valve positioning pin hole 115, forms sealing with the upper surface of the main body module 100 through an air-filled sealing valve sealing gasket 306, and is fixed on the upper surface of the main body module 100 through the air-filled sealing valve fixing threaded hole 113;
the air outlet hole 120 of the air-charging quantitative pulse valve and the air inlet hole 121 of the air-charging quantitative pulse valve are symmetrically provided with the fixed threaded hole 122 of the air-charging quantitative pulse valve and the positioning pin hole 123 of the air-charging quantitative pulse valve, the air-charging quantitative pulse valve 308 is positioned on the front surface of the main body module 100 through the positioning pin hole 123 of the air-charging quantitative pulse valve, forms a seal with the front surface of the main body module 100 through the sealing pad 307 of the air-charging quantitative pulse valve, and is fixed on the front surface of the main body module 100 through the fixed threaded hole 122 of the air-charging quantitative pulse valve;
The air outlet hole 131 and the air inlet hole 133 of the air extraction quantitative pulse valve are symmetrically provided with the fixed threaded hole 129 of the air extraction quantitative pulse valve and the positioning pin hole 130 of the air extraction quantitative pulse valve on both sides of the whole body, the air extraction quantitative pulse valve 309 is positioned on the front surface of the main body module 100 through the positioning pin hole 130 of the air extraction quantitative pulse valve, forms a seal with the front surface of the main body module 100 through the sealing gasket 310 of the air extraction quantitative pulse valve, and is fixed on the front surface of the main body module 100 through the fixed threaded hole 129 of the air extraction quantitative pulse valve;
sample tube fixing threaded holes 127 are symmetrically formed around the sample tube interface mounting groove 149, and the sample tube module is fixed on the lower surface of the main body module 100 through the sample tube fixing threaded holes 127.
As shown in fig. 4, the sample tube module includes a sample tube 200, a sample tube lock nut 201, a sample tube lock nut combination seal ring 204, a sample tube lock nut O-ring 205, a sample tube interface 206 and a sample tube interface O-ring 210,
the center of the sample tube lock nut 201 is provided with a sample tube lock nut center hole 202, the upper surface of the sample tube lock nut 201 is provided with a sample tube lock nut platform 203, a sample tube lock nut combined sealing ring 204 and a sample tube lock nut O-shaped ring 205 are placed on the sample tube lock nut platform 203 from bottom to top, the sample tube lock nut is installed inside a sample tube interface 206, the center of the sample tube interface 206 is provided with a sample tube interface center hole 207, the surface of the sample tube interface 206 is symmetrically provided with a sample tube interface through hole 209, the center of the upper surface of the sample tube interface 206 is provided with a sample tube interface O-shaped ring placing groove 208, the sample tube interface O-shaped ring placing groove 208 is internally provided with a sample tube interface O-shaped ring 210, the sample tube interface 206 is fixed on the lower surface of the main body module 100 through a sample tube fixing threaded hole 127 and the sample tube lock nut 201, the sample tube lock nut combined sealing ring 204 and the sample tube lock nut O-shaped ring 205, and the sample tube lock nut O-shaped ring 205 are fastened through the sample tube lock nut O-shaped ring 205, and the sample tube interface O-shaped ring 205 is compressed by the fastening nut 205 in the radial direction;
The enclosed volume enclosed by the sample tube sealing valve vent hole 110, the sample tube connecting aperture 128, the sample tube sealing valve vent aperture 148, and the sample tube 200 on the body module 100 is referred to as a sample chamber;
the enclosed volume enclosed by the air suction three-way valve air inlet 104, the air pressure sensor sealing ring placing groove 107, the sample tube sealing valve air inlet 111, the air inflation sealing valve air outlet 114 and the reference cavity cover plate 162 is called a reference cavity.
The air path sealing module comprises a vacuum pump regulating valve 165, a vacuum pump combined sealing ring 164, an external air source clamping sleeve joint 160, an external air source combined sealing ring 159, a reference cavity sealing O-ring 161 and a reference cavity cover plate 162,
the reference cavity sealing O-ring 161 is placed in the reference cavity sealing ring placing groove 146, an end face seal is formed by compressing the reference cavity cover plate 162, an inflatable filter 158 is placed at the joint of the external air source air inlet coarse pore channel 118 and the external air source air inlet fine pore channel 117, the external air source clamping sleeve joint 160 is fixed on the right side surface of the main body module 100 through threads in the external air source air inlet hole 119, the external air source combined sealing ring 159 is compressed to form a seal, and the inflatable filter 158 is compressed through the external air source combined sealing ring 159;
the vacuum pump regulating valve 165 is fixed on the left side surface of the main body module 100 through threads in the air extraction pipeline connector 138, and compresses the vacuum pump assembly sealing ring 164 to form a seal;
Four reference cavity cover plate through holes 163 are symmetrically formed in the periphery of the reference cavity cover plate 162, reference cavity cover plate fixing threaded holes 125 are symmetrically formed in the periphery of the reference cavity cover plate placing groove 124, fastening screws are screwed into the reference cavity cover plate fixing threaded holes 125 through the four reference cavity cover plate through holes 163 to be fixed on the right side surface of the main body module 100, and a reference cavity sealing O-shaped ring 161 is placed in the reference cavity sealing ring placing groove 146.
The valve module comprises an air extraction three-way valve 301, an air extraction three-way valve sealing ring 302, a sample tube sealing valve 303, a sample tube sealing valve sealing gasket 304, an air inflation sealing valve 305, an air inflation sealing valve sealing gasket 306, an air inflation quantitative pulse valve 308, an air inflation quantitative pulse valve sealing gasket 307, an air extraction quantitative pulse valve 309 and an air extraction quantitative pulse valve sealing gasket 310, wherein the valves of the valve module are all seat-mounted electromagnetic valves, and are sealed with a smooth plane through the sealing gaskets;
as shown in fig. 6, the lower surface of the air extraction three-way valve 301 is horizontally provided with an air extraction three-way valve fixing through hole 317, an air extraction three-way valve through air outlet 318, an air extraction three-way valve pulsation air outlet 319, an air extraction three-way valve air inlet 320 and an air extraction three-way valve positioning pin 322, the lower surface of the air extraction three-way valve 301 is provided with an air extraction three-way valve sealing groove 321, and the air extraction three-way valve sealing gasket 302 is placed in the air extraction three-way valve sealing groove 321; when the air extraction three-way valve 301 is in a closed state, the air inlet 320 of the air extraction three-way valve is communicated with the through air outlet 318 of the air extraction three-way valve, and the air inlet 320 of the air extraction three-way valve is blocked from the pulsating air outlet 319 of the air extraction three-way valve; when the air extraction three-way valve 301 is in an open state, the air inlet 320 of the air extraction three-way valve is blocked from the through air outlet 318 of the air extraction three-way valve, and the air inlet 320 of the air extraction three-way valve is communicated with the pulsation air outlet 319 of the air extraction three-way valve;
As shown in fig. 5, the lower surface center of the air extraction quantitative pulse valve 309 is symmetrically provided with an air extraction quantitative pulse valve fixing through hole 311 and an air extraction quantitative pulse valve positioning pin 316, the center of the lower surface of the air extraction quantitative pulse valve 309 is provided with an air extraction quantitative pulse valve expansion port 313, two sides of the air extraction quantitative pulse valve expansion port 313 are symmetrically provided with an air extraction quantitative pulse valve air inlet 312 and an air extraction quantitative pulse valve air outlet 314, the lower surface of the air extraction quantitative pulse valve 309 is provided with an air extraction quantitative pulse valve sealing groove 315, and the air extraction quantitative pulse valve sealing gasket 310 is placed in the air extraction quantitative pulse valve sealing groove 315; when the air extraction quantitative pulse valve 309 is in an open state, the air extraction quantitative pulse valve air inlet 312 and the air extraction quantitative pulse valve air outlet 314 are alternately opened and closed at the frequency of 10 Hz, the air between the air extraction quantitative pulse valve air inlet 312 and the air extraction quantitative pulse valve air outlet 314 is discharged, and when the air extraction quantitative pulse valve 309 is in a closed state, the air extraction quantitative pulse valve air inlet 312 is kept sealed to block the air;
as shown in fig. 7, a sample tube sealing valve fixing through hole 323 and a sample tube sealing valve positioning pin 324 are symmetrically arranged at the center of the lower surface of the sample tube sealing valve 303, a sample tube sealing valve air inlet 325 is formed at the center of the lower surface of the sample tube sealing valve 303, a sample tube sealing valve air outlet 326 is formed beside the sample tube sealing valve air inlet 325, a sample tube sealing valve sealing groove 327 is formed at the lower surface of the sample tube sealing valve 303, and a sample tube sealing valve sealing gasket 304 is placed in the sample tube sealing valve sealing groove 327; when the sample tube sealing valve 303 is in an open state, the sample tube sealing valve air inlet 325 is communicated with the sample tube sealing valve air outlet 326; when the sample tube sealing valve 303 is in a closed state, the sample tube sealing valve air inlet 325 is blocked from the sample tube sealing valve air outlet 326;
As shown in fig. 8, two fixed through holes 328 and locating pins 333 are symmetrically arranged at the center of the lower surface of the quantitative air pulse valve 308, an expansion port 330 is arranged at the center of the lower surface of the quantitative air pulse valve 308, an air outlet 329 and an air inlet 331 are symmetrically arranged at two sides of the expansion port 330, a sealing groove 332 is arranged, and a sealing pad 307 is arranged in the sealing groove 332; when the quantitative inflation pulse valve 308 is in an open state, the quantitative inflation pulse valve air inlet 331 and the quantitative inflation pulse valve air outlet 329 are alternately opened and closed at a frequency of 10Hz, and the gas between the quantitative inflation pulse valve air inlet 331 and the quantitative inflation pulse valve air outlet 329 is discharged; when the quantitative inflation pulse valve 308 is in a closed state, the quantitative inflation pulse valve air inlet 331 is kept sealed to block air;
as shown in fig. 9, two inflation sealing valve fixing through holes 334 and an inflation sealing valve positioning pin 335 are symmetrically arranged at the center of the lower surface of the inflation sealing valve 305, an inflation sealing valve air outlet 336 is formed at the center of the lower surface of the inflation sealing valve 305, an inflation sealing valve air inlet 337 is formed beside the inflation sealing valve air outlet 336, an inflation sealing valve sealing groove 338 is formed at the lower surface of the inflation sealing valve 305, and an inflation sealing valve sealing gasket 306 is placed in the inflation sealing valve sealing groove 338; when the inflation sealing valve 305 is in an open state, the inflation sealing valve air inlet 337 is communicated with the inflation sealing valve air outlet 336; when the air-packing valve 305 is in the closed state, the air-packing valve air inlet 337 is blocked from the air-packing valve air outlet 336.
The air extraction three-way valve positioning pin 322 on the air extraction three-way valve 301 is aligned with the air extraction three-way valve positioning pin hole 105 on the main body module 100, the air extraction three-way valve through air outlet 318 on the air extraction three-way valve 301 is communicated with the air extraction three-way valve through air outlet hole 102 on the main body module 100, the air extraction three-way valve pulsation air outlet 319 on the air extraction three-way valve 301 is communicated with the air extraction three-way valve pulsation air outlet hole 103 on the main body module 100, the air extraction three-way valve air inlet 320 on the air extraction three-way valve 301 is communicated with the air extraction three-way valve air inlet hole 104 on the main body module 100, the fastening screw is screwed into the air extraction three-way valve fixing threaded hole 101 on the main body module 100 through the air extraction three-way valve fixing through hole 317 on the air extraction three-way valve 301, and after the fastening screw is screwed, the air extraction three-way valve 301 and the main body module 100 form a seal;
the air-charging quantitative pulse valve locating pin 333 on the air-charging quantitative pulse valve 308 is aligned with the air-charging quantitative pulse valve locating pin hole 123 on the main body module 100, the air-charging quantitative pulse valve air outlet 329 on the air-charging quantitative pulse valve 308 is communicated with the air-charging quantitative pulse valve air outlet hole 120 on the main body module 100, the air-charging quantitative pulse valve expanding opening 330 on the air-charging quantitative pulse valve 308 is communicated with the air-charging quantitative pulse valve expanding hole 142 on the main body module 100, the air-charging quantitative pulse valve air-inlet 331 on the air-charging quantitative pulse valve 308 is communicated with the air-charging quantitative pulse valve air-charging hole 121 on the main body module 100, the fastening screw is screwed into the air-charging quantitative pulse valve fixing threaded hole 122 on the main body module 100 through the air-charging quantitative pulse valve fixing through hole 328 on the air-charging quantitative pulse valve 308, and after the fastening screw is screwed, the air-charging quantitative pulse valve 308 forms a seal with the main body module 100;
The air extraction quantitative pulse valve positioning pin 316 on the air extraction quantitative pulse valve 309 is aligned with the air extraction quantitative pulse valve positioning pin hole 130 on the main body module 100, the air extraction quantitative pulse valve air inlet 312 on the air extraction quantitative pulse valve 309 is communicated with the air extraction quantitative pulse valve air inlet hole 133 on the main body module 100, the air extraction quantitative pulse valve expansion opening 313 on the air extraction quantitative pulse valve 309 is communicated with the air extraction quantitative pulse valve expansion hole 157 on the main body module 100, the air extraction quantitative pulse valve air outlet 314 on the air extraction quantitative pulse valve 309 is communicated with the air extraction quantitative pulse valve air outlet hole 131 on the main body module 100, the fastening screw is screwed into the air extraction quantitative pulse valve fixing threaded hole 129 on the main body module 100 through the air extraction quantitative pulse valve fixing through hole 311 on the air extraction quantitative pulse valve 309, and after the fastening screw is screwed, the air extraction quantitative pulse valve 309 and the main body module 100 form a seal;
the sample tube sealing valve positioning pin 324 on the sample tube sealing valve 303 is aligned with the sample tube sealing valve positioning pin hole 112 on the main body module 100, the sample tube sealing valve air inlet 325 on the sample tube sealing valve 303 is communicated with the sample tube sealing valve air inlet 111 on the main body module 100, the sample tube sealing valve air outlet 326 on the sample tube sealing valve 303 is communicated with the sample tube sealing valve air outlet 110 on the main body module 100, the fastening screw is screwed into the sample tube sealing valve fixing threaded hole 109 on the main body module 100 through the sample tube sealing valve fixing through hole 323 on the sample tube sealing valve 303, and after the fastening screw is screwed, the sample tube sealing valve 303 forms a seal with the main body module 100;
The air-filled sealing valve positioning pin 335 on the air-filled sealing valve 305 is aligned with the air-filled sealing valve positioning pin hole 115 on the main body module 100, the air-filled sealing valve air inlet 337 on the air-filled sealing valve 305 is communicated with the air-filled sealing valve air inlet 116 on the main body module 100, the air-filled sealing valve air outlet 336 on the air-filled sealing valve 305 is communicated with the air-filled sealing valve air outlet 114 on the main body module 100, the fastening screw is screwed into the air-filled sealing valve fixing threaded hole 113 on the main body module 100 through the air-filled sealing valve fixing through hole 334 on the air-filled sealing valve 305, and after the fastening screw is screwed, the air-filled sealing valve 305 forms a seal with the main body module 100.
In a specific test, the following steps are performed:
s1, filling an adsorbent: unscrewing the sample tube lock nut 201, removing the sample tube 200, and weighing the mass m of the sample tube 200 t After the adsorbent to be tested is filled, the total mass m of the sample tube 200 and the adsorbent is weighed s Inserting the sample tube 200 into the sample tube interface 206, screwing the sample tube locking nut 201 to finish the filling of the adsorbent, placing the sample tube 200 containing the adsorbent into the liquid adsorbent, and closing all valves;
s2, cleaning the reference cavity and the sample cavity: the external air source is switched to high-purity argon, an external vacuum pump is opened, a vacuum pump regulating valve 165 is regulated, an air suction three-way valve 301 is closed and switched to an air flow through state, a reference cavity is vacuumized, a sample tube sealing valve 303 is opened after 10 seconds to vacuumize the sample cavity, the reference cavity and the air in the sample cavity are connected with a pore 128 through a sample tube, an air outlet pore 148 of the sample tube sealing valve, the sample tube sealing valve 303, an air inlet pore 151 of the sample tube sealing valve, a main pore 126 of the reference cavity, an air suction three-way valve air inlet pore 132, an air suction three-way valve 301, an air suction three-way valve through air outlet pore 140, a vacuum pump air suction fine pore 136, a vacuum pump air suction coarse pore 137 and a vacuum pump regulating valve 165 are discharged, an air pressure sensor 406 is opened and switched to an air flow closing state when the pressure is lower than 0.001 Pa, opening an inflation sealing valve 305, filling argon into a reference cavity and a sample cavity, enabling the argon to enter the main body module 100 through an external air source clamping sleeve joint 160, enabling the argon to enter an external air source air inlet rough pore channel 118 and an inflation filter piece 158 to enter an external air source air inlet fine pore channel 117, an inflation sealing valve air inlet pore channel 141, an inflation sealing valve 305 and an inflation sealing valve air outlet pore channel 143 to enter a reference cavity main pore channel 126, enabling part of the argon in the reference cavity main pore channel 126 to enter a pressure sensor core seat 108, enabling the other part of the argon to enter a sample tube sealing valve air inlet pore channel 151, a sample tube sealing valve 303 and a sample tube sealing valve air outlet pore channel 148, enabling the argon to enter the sample tube 200 through a sample tube connecting pore channel 128, closing the inflation sealing valve 305 when the pressure value measured by a pressure sensor 406 reaches 27-30 kPa, and closing the sample tube sealing valve 303 after 10 seconds, so as to finish one-time cleaning;
S3, air volume calibration: repeating the step S2 four times to finish the replacement cleaning of the reference cavity and the sample cavity; the three-way valve 301 is closed to switch to an air flow through state, the reference cavity is vacuumized, the sample tube sealing valve 303 is opened to vacuumize the sample cavity after 10 seconds, the reference cavity and the gas in the sample cavity are connected with the pore 128 through the sample tube, the sample tube sealing valve air outlet pore 148, the sample tube sealing valve 303, the sample tube sealing valve air inlet pore 151, the reference cavity main pore 126, the three-way valve air inlet pore 132, the three-way valve 301, the three-way valve air outlet pore 140, the vacuum pump air outlet fine pore 136, the vacuum pump air outlet coarse pore 137 and the vacuum pump regulating valve 165 are opened, the air pressure sensor 406 measures the pressure of the gas, when the pressure is lower than 0.001 and Pa, the vacuum environment is considered, the three-way valve 301 is opened to switch to an air flow closing state, and the pressure P is measured and recorded through the air pressure sensor 406 after 10 seconds b Closing a sample tube sealing valve 303, opening an inflation sealing valve 305 to charge argon into a reference cavity, enabling the argon to enter the main body module 100 through an external air source clamping sleeve joint 160, enabling an external air source air inlet rough duct 118, an inflation filter piece 158, an external air source air inlet fine duct 117, an inflation sealing valve air inlet duct 141, an inflation sealing valve 305 and an inflation sealing valve air outlet duct 143 to enter a reference cavity main duct 126, enabling part of the argon in the reference cavity main duct 126 to enter a pressure sensor core seat 108, enabling the other part of the argon to enter a sample tube sealing valve air inlet duct 151, closing the inflation sealing valve 305 when the pressure sensor 406 detects that the pressure is 27-30 kPa, and measuring and recording the pressure value P at the moment after 10 seconds in Opening the sample tube sealing valve 303, allowing argon to enter the sample tube 200 through the sample tube sealing valve 303, the sample tube sealing valve air outlet pore 148 and the sample tube connecting pore 128, monitoring the gas pressure in real time by the gas pressure sensor 406, and measuring and recording the gas pressure value P at the moment after 10 seconds eq The method comprises the steps of carrying out a first treatment on the surface of the Argon is not absorbed by the adsorbent material, i.e. the mole number of argon is unchanged, the air pressure changes corresponding to the volume changes, and passes through the sample tube sealing valve 303 before and after opening the air pressure value and the reference cavity volume V r Calculating to obtain the free volume V of the sample tube 200 after the sample is added f The method comprises the following steps:
s4, measuring adsorption data points at low pressure: closing a sample tube sealing valve 303, starting a vacuum pump, closing an air suction three-way valve 301, switching to an air flow through state, vacuumizing a reference cavity, opening the sample tube sealing valve 303 after 10 seconds, vacuumizing the sample cavity, discharging argon in the reference cavity and the sample cavity through an air suction three-way valve air inlet channel 132, an air suction three-way valve 301, an air suction three-way valve through air outlet channel 140, a vacuum pump air suction fine channel 136, a vacuum pump air suction coarse channel 137 and a vacuum pump regulating valve 165, measuring the air pressure by an air pressure sensor 406, opening the air suction three-way valve 301, switching to an air flow closing state when the pressure is lower than 0.001 Pa, and measuring the pressure P at the moment after 10 seconds 1,b Closing the sample tube sealing valve 303, connecting the external air source clamping sleeve joint 160 with a high-purity adsorbate gas bottle, opening the air inflation sealing valve 305, filling adsorbate into the reference cavity, enabling the adsorbate to enter the main body module 100 through the external air source clamping sleeve joint 160, enabling the external air source to enter the rough air channel 118, the air inflation filter 158, the external air source to enter the fine air channel 117, the air inflation sealing valve air inlet channel 141, the air inflation sealing valve 305 and the air inflation sealing valve air outlet channel 143 to enter the reference cavity main channel 126, enabling the adsorbate in the reference cavity main channel 126 to be divided into two flow directions, enabling one part of adsorbate to enter the air pressure sensor core seat 108, enabling the other part of adsorbate to enter the sample tube sealing valve air inlet channel 151, and when the air pressure sensor 406 detects that the air pressure is 1kPa of a first adsorption data point pressure, closing the air inflation sealing valve 305, measuring and recording the pressure value P after 10 seconds 1,in The sample tube sealing valve 303 was opened and the pressure value P was measured and recorded after 10 seconds 1,eq The method comprises the steps of carrying out a first treatment on the surface of the Given that the dynamic viscosity of the adsorbate is μ, the thickness of the air-filled filter sheet 158 is H, the permeability is k, and the diameter of the gas passing through the air-filled filter sheet 158 is D, the gas passes through the air-filled filter sheet 158 and then toward the reference chamber V r Minimum time t required for permeation of adsorbate min And the longest time t max The method comprises the following steps of:
Wherein DeltaP min And DeltaP max The minimum and maximum values of the absolute pressure in the sample cavity and the pressure difference at the external air source ferrule fitting 160, respectively;
first adsorption equilibrium pressure P 1,eq Number n of moles of adsorbent adsorbed by the corresponding adsorbent 1 The method comprises the following steps:
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s5, measuring adsorption data points at high pressure: each time to the reference chamber i,inlet When the pressure sensor 406 detects that the pressure in the main pore canal 126 of the reference cavity is greater than 25 kPa and the pressure sensor monitors that the pressure in the main pore canal 126 of the reference cavity is greater than 25 kPa, the time required for air intake of the air filter 158 is increased, so that the air leakage of the sample cavity and the reference cavity is increased, at the moment, the air intake of the air intake quantitative pulse valve 308 is switched to, the air intake quantitative pulse valve 308 can enter 0.05 mL air each time, the working frequency of the air intake quantitative pulse valve 308 is 10 Hz, and the pressure P in the i-1 time of balance is passed i-1,eq The number of moles of the corresponding adsorption is n i-1 Reference chamber volume V r The pressure P at the external air source cutting sleeve joint 160 calculates the required time t seconds, the adsorbate enters the main body module 100 through the external air source cutting sleeve joint 160, enters the air pressure sensor core seat 108 through the external air source air inlet rough pore canal 118, the air charging quantitative pulse valve air inlet pore canal 145, the air charging quantitative pulse valve 308, the air charging quantitative pulse valve air outlet pore canal 144, the external air source air inlet fine pore canal 117, the air charging sealing valve air inlet pore canal 141, the air charging sealing valve 305, the air charging sealing valve air outlet pore canal 143 and enters the reference cavity main pore canal 126, the adsorbate in the reference cavity main pore canal 126 is divided into two flow directions, one part of adsorbate enters the air pressure sensor core seat 108, and the other part of adsorbate enters the sample tube sealing valve The inflation is completed after t seconds in the air hole channel 151, and the calculation process of t is as follows:
the charge metering pulse valve 308 needs to be switched x times:
the operating time t of the charge metering pulse valve 308 is:
t = x ÷ 10
the inflation sealing valve 305 is closed, and the air pressure value P at this time is measured and recorded after 10 seconds i,in The sample tube sealing valve 303 was opened, and the air pressure value P was measured and recorded after 10 seconds i,eq Ith adsorption equilibrium pressure P i,eq Number n of moles of adsorbent adsorbed by the corresponding adsorbent i The method comprises the following steps:
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s6, repeating the step S5 until the air pressure sensor 406 detects that the pressure in the reference cavity reaches a standard atmospheric pressure, stopping measuring adsorption data, and drawing an isothermal adsorption line at the temperature according to the measurement result;
s7, determination of desorption data points at high pressure: the isothermal desorption line is measured by adopting the state at the end of the adsorption process as the initial state, all valves are closed, the sample tube containing the adsorbent is still placed in the temperature environment where the adsorbent is positioned during adsorption, and the absolute pressure at the air exhaust pipeline interface 138 is close to 0 kPa; at this time, the pressure in the reference cavity is P 0,eq The mole number of the adsorption mass is n 0,de . At this time, the pressure difference between the pressure in the reference cavity and the pressure at the air extraction pipeline interface 138 is too large, the pressure in the reference cavity can be changed too fast through direct air extraction, and the air pressure sensor 406 is used for measuring lag to cause untimely feedback of the air extraction three-way valve 301, so that air extraction is performed by adopting the air extraction quantitative pulse valve 309; the three-way valve 301 is switched to the air flow closing state, the quantitative pulse valve 309 is opened to pump air to the reference cavity, the quantitative pulse valve 309 can enter 0.05 mL gas each time, and the pressure in the reference cavity is adjusted to P when the first desorption data point is measured 1,outlet According to the referenceCavity volume V r The operation frequency of the air extraction quantitative pulse valve 309 is 10 Hz, and the required time t seconds can be calculated by the following calculation process:
the bleed air metering pulse valve 309 needs to be switched x times:
the operating time t of the bleed air dosing pulse valve 309 is:
t = x ÷ 10
the adsorbate gas in the main pore 126 of the reference cavity is discharged through the air inlet pore 132 of the air suction three-way valve, the air suction three-way valve 301, the pulsating air outlet pore 139 of the air suction three-way valve, the air inlet pore 134 of the air suction quantitative pulse valve, the air suction quantitative pulse valve 309, the air outlet pore 135 of the air suction quantitative pulse valve, the vacuum pump air suction fine pore 136, the vacuum pump air suction coarse pore 137 and the vacuum pump regulating valve 165, after the time t, the air suction is completed, the air suction quantitative pulse valve 309 is closed, and after 10 seconds, the air pressure value P at the moment is measured and recorded 1,out The sample tube sealing valve 303 was opened and the pressure value P was measured and recorded after 10 seconds 1,eq First desorption equilibrium pressure P 1,eq Number n of moles of adsorbent adsorbed by the corresponding adsorbent 1,de The method comprises the following steps:
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s8, measuring desorption data points at low pressure: each time the air is pumped from the reference cavity by 5 kPa lower than the last balance pressure, when the balance pressure is lower than the absolute pressure by 25 kPa, the pressure difference between the inside and outside of the air pumping quantitative pulse valve 309 is too small, the time required for pumping by using the air pumping quantitative pulse valve 309 is increased, the air leakage of the sample cavity and the reference cavity is increased, and at the moment, the air pumping three-way valve 301 is required to be closed to be switched to an air flow through state for pumping; pressure at the i-1 st equilibrium is P i-1,eq The corresponding adsorption quantity is n i-1,de Closing the sample tube sealing valve 303, closing the air extraction three-way valve 301, switching to an air flow through state to extract air from the reference cavity, and allowing air in the main pore canal 126 of the reference cavity to pass throughThe air inlet channel 132 of the air three-way valve, the air extraction three-way valve 301, the air extraction three-way valve direct air outlet channel 140, the vacuum pump air extraction fine channel 136, the vacuum pump air extraction coarse channel 137 and the vacuum pump regulating valve 165 are discharged, when the air pressure sensor 406 detects that the pressure value reaches the preset pressure +/-1 kPa, the air extraction three-way valve 301 is opened to switch to the air flow closing state to stop air extraction, and after 10 seconds, the pressure P is measured and recorded i,out The sample tube sealing valve 303 was opened and after 10 seconds the pressure was measured and recorded as P i,eq Then the ith desorption equilibrium pressure P i,eq Number n of moles of adsorbent adsorbed by the corresponding adsorbent i,de The method comprises the following steps:
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s9, repeating the steps S7 and S8 until the pressure sensor 406 detects that the pressure is lower than the absolute pressure of 0.001 and Pa, stopping measuring desorption data, and drawing an isothermal desorption line at the temperature according to the measurement result;
s10, residual gas treatment: the sample tube sealing valve 303 is opened, the air extraction three-way valve 301 is closed to be switched to an air flow through state, and air in the sample cavity and the reference cavity is discharged through the air extraction three-way valve air inlet pore canal 132, the air extraction three-way valve 301, the air extraction three-way valve through air outlet pore canal 140, the vacuum pump air suction fine pore canal 136, the vacuum pump air suction coarse pore canal 137 and the vacuum pump regulating valve 165, the air pressure is measured by the air pressure sensor 406, and when the pressure is smaller than 0.001 Pa, the air extraction three-way valve 301 is opened to be switched to an air flow closing state to stop air extraction.
Example 1
Weigh empty sample cell mass m t 7.7715 g, the total mass m of the empty sample tube and the activated carbon is weighed after the activated carbon is filled into the test sample s 7.9142 g the mass of the activated carbon is m c For 0.1427 g, the sample tubes containing activated carbon adsorbent were placed in a 77.35K liquid nitrogen bath with all valves closed.
(1) Washing the reference chamber and the sample chamber 5 times
A. The external air source adopts high-purity argon, the pressure at the air inlet hole of the external air source is adjusted to be 140+/-1 kPa, an external vacuum pump is opened, a regulating valve of the vacuum pump is regulated, and an air extraction three-way valve is opened to be switched to an air flow closing state;
B. closing the air extraction three-way valve, switching to an air flow through state, vacuumizing the reference cavity, opening the sample tube sealing valve after 10 seconds, and vacuumizing the sample cavity;
C. when the pressure reaches below 0.001 and Pa, the air extraction three-way valve is opened to switch to an air flow closing state;
D. opening an inflation sealing valve, filling argon into the reference cavity and the sample cavity, closing the inflation sealing valve when the pressure value of the air pressure sensor reaches 27-30 kPa, and closing the sample tube sealing valve after 10 seconds to finish the first cleaning;
E. and (3) repeating the steps B-D four times to finish the replacement cleaning of the reference cavity and the sample cavity.
(2) Measuring the free volume V of the sample tube f
A. Switching the air extraction three-way valve to an air flow through state, vacuumizing the reference cavity, opening the sample tube sealing valve after 10 seconds, vacuumizing the sample cavity, opening the air extraction three-way valve to be switched to an air flow closing state when the pressure reaches below 0.001 Pa, and measuring the pressure after 10 seconds, wherein the value P of the pressure is the value P b 0.015 to Pa, closing the sample tube sealing valve;
B. opening an inflation sealing valve, filling argon into the reference cavity, closing the inflation sealing valve when the pressure value of the air pressure sensor reaches 27-30 kPa, and measuring the pressure after 10 seconds, wherein the value P is the value in 30.025 kPa;
C. the sample tube sealing valve is opened, and the pressure is measured after 10 seconds, and the value P of the pressure is measured eq Known as reference cavity volume V at 27.961 kPa r 119.6 mL, the empty volume V of the sample cavity is filled with the adsorbent activated carbon f The method comprises the following steps:
(3) Determination of the first adsorption data point of the isothermal adsorption line
The first adsorption data point of the isothermal adsorption line refers to the first adsorption equilibrium pressure P from low pressure 1,eq P 1,eq Corresponding mole number of active carbon adsorption nitrogenn 1 . And replacing the external air source with high-purity nitrogen, and adjusting the pressure at the clamping sleeve joint of the external air source to be 140+/-1 kPa. When the pressure in the sample cavity is lower than the absolute pressure of 25 kPa, the air inflation quantitative pulse valve cannot work, and at the moment, the air intake time is prolonged by utilizing the air inflation filter. Absolute pressure in the sample cavity is set to be 0.001 Pa and 25 kPa respectively, and the absolute pressure is different from the pressure 140 kPa at the external air source cutting sleeve joint by a minimum delta P min And a maximum value DeltaP max The method comprises the following steps of:
ΔP min = 140 – 25 = 115 kPa
ΔP max = 140 – 0.000001 ≈ 140 kPa
the dynamic viscosity of nitrogen is 17.805 multiplied by 10 -6 Pa.s, thickness H of the inflatable filter membrane is 2 mm, and volume V of the reference cavity r 119.6. 119.6 mL, a permeability k of 5.43X 10 -13 m 2 The diameter D of the gas passing through the gas-filled filter sheet is 3 mm, and the gas passes through the gas-filled filter sheet and then flows into the reference cavity V r Minimum time t required for nitrogen permeation min And the longest time t max The method comprises the following steps of:
the feedback time of the inflation sealing valve is 0.5 second and is less than t min And t max It is illustrated that the inflatable sealing valve has enough feedback time to open and close to control the pressure of the gas entering the reference chamber.
A. Switching the air extraction three-way valve to an air flow through state, vacuumizing the reference cavity, opening the sample tube sealing valve after 10 seconds, vacuumizing the sample cavity, opening the air extraction three-way valve to be switched to an air flow closing state when the pressure reaches below 0.001 Pa, and measuring the pressure after 10 seconds, wherein the value P of the pressure is the value P 1,b For 0.017 Pa, closing the sample tube sealing valve;
B. opening an inflation sealing valve, filling nitrogen into the reference cavity, and closing the inflation when the pressure value of the air pressure sensor reaches 0.730 kPaAir-tight valve, measuring pressure after 10 seconds, value P thereof 1,in 0.732 kPa;
C. the sample tube sealing valve is opened, and the pressure is measured after 10 seconds, and the value P of the pressure is measured 1,eq A universal gas constant R of 8.314J. Mol at 0.017 kPa -1 ·K -1 The liquid nitrogen bath temperature T is 77.35K, the first adsorption equilibrium pressure P 1,eq Corresponding mole number n of active carbon adsorption nitrogen 1 The method comprises the following steps:
D. equilibrium pressure P of the first adsorption data point of isothermal adsorption line 1,eq The molar number n of the nitrogen adsorbed by the activated carbon is 0.017 kPa 1 Is 0.133×10 -3 mol。
(4) Determination of the second adsorption data point of the isothermal adsorption line
A. Closing the sample tube sealing valve, opening the inflation sealing valve, filling nitrogen into the reference cavity, closing the inflation sealing valve when the pressure value of the air pressure sensor reaches 0.780 kPa, and measuring the pressure after 10 seconds, wherein the value P is the value 2,in Is 0.782 kPa;
B. the sample tube sealing valve is opened, and the pressure is measured after 10 seconds, and the value P of the pressure is measured 2,eq At 0.148 kPa, the second adsorption equilibrium pressure P 2,eq Corresponding mole number n of active carbon adsorption nitrogen 2 The method comprises the following steps:
C. equilibrium pressure P of the first adsorption data point of isothermal adsorption line 2,eq The molar number n of the nitrogen adsorbed by the activated carbon is 0.148 kPa 2 Is 0.249×10 -3 mol。
(5) Determination of isothermal adsorption line ith adsorption data point
When the balance pressure exceeds 25 kPa, the time required for air intake by the filter is increased, so that the air leakage of the sample cavity and the reference cavity is increased, and the switching is needed at the momentAnd (5) air is fed into the air charging quantitative pulse valve. Setting the pressure P of the i-1 th time balance i-1,eq 70 kPa, the pressure after gas filling is 75 kPa, corresponding to the adsorption quantity n i-1 1.461×10 -3 The mol, the aeration quantitative pulse valve can enter 0.05 mL gas each time, the air enters a reference cavity V with the volume of 119.6 mL r The nitrogen filling of 140 kPa needs to be turned on and off x times and the calculation process is as follows:
A. the operating frequency of the charge metering pulse valve is 10 Hz, and it takes 184++10=18.4 seconds to complete the charge. The quantitative pulse valve for aeration is closed, the pressure is measured after 10 seconds, and the value P of the quantitative pulse valve for aeration is measured i,in 75.2 kPa;
B. the sample tube sealing valve is opened, and the pressure is measured after 10 seconds, and the value P of the pressure is measured i,eq 71.515 kPa, the ith adsorption equilibrium pressure P i,eq Corresponding mole number n of active carbon adsorption nitrogen i The method comprises the following steps:
C. equilibrium pressure P of ith adsorption data point of isothermal adsorption line i,eq The molar number n of the nitrogen adsorbed by the activated carbon is 71.515 kPa i 2.126 ×10 -3 mol。
Repeating the above aeration measurement steps until the pressure reaches a standard atmospheric pressure, stopping measuring adsorption data, and drawing an isothermal adsorption line of the activated carbon for adsorbing nitrogen according to the measurement result.
Example 2
Isothermal desorption lines of the activated carbon desorbed nitrogen were drawn by isothermal desorption data. The isothermal desorption line was measured using the state at the end of the adsorption process in example 1 as the initial state, the sample tube containing the activated carbon adsorbent was still placed in a 77.35K liquid nitrogen bath, the absolute pressure at the interface of the suction line was approximately 0 kPa, and the mass m of the activated carbon adsorbent was known from example 1 c 0.1427 g reference Chamber volume V r 119.6. 119.6 mL, sample cavityVoid volume V f 8.8 mL, the number of moles n of nitrogen adsorbed at the end of the adsorption process 0,de Is 2.39X10 -3 mol, at this time reference intra-cavity pressure P 0,eq All valves were closed at 100.847 kPa.
(1) Determination of the first desorption data point of the isothermal desorption line
The first desorption data point of the isothermal desorption line refers to the first adsorption equilibrium pressure P from high pressure 1,eq P 1,eq Corresponding mole number n of active carbon desorption nitrogen 1,de . At the moment, the pressure difference at the interface of the pressure in the reference cavity and the air extraction pipeline is too large, the pressure in the reference cavity can be changed too fast through direct air extraction, and the three-way valve for air extraction is not fed back timely due to measurement lag of the pressure sensor, so that the air extraction quantitative pulse valve for air extraction is adopted.
A. Opening the sealing valve of the sample tube, and measuring the initial equilibrium pressure P in the desorption process after 10 seconds 0,eq For 100.847 kPa, the sample tube sealing valve is closed, and the pressure P in the cavity is referenced 1,out Adjusting to 92.5 kPa, opening an air extraction three-way valve, switching to an air flow closing state, opening an air extraction quantitative pulse valve to extract air from the reference cavity, wherein the air extraction quantitative pulse valve can extract 0.05 mL air each time, and the vacuum pump is connected with the reference cavity V with the volume of 119.6 mL through the air extraction quantitative pulse valve r When the gas is pumped out, the pumping quantitative pulse valve needs to be opened and closed for x times, and the calculation process is as follows:
B. the operating frequency of the bleed pulse valve was 10 Hz, requiring 216+.10=21.6 seconds to complete the bleed. Closing the air extraction quantitative pulse valve, measuring pressure after 10 seconds, and measuring the value P 1,out 92.504 kPa;
C. the sample tube sealing valve is opened, and the pressure is measured after 10 seconds, and the value P of the pressure is measured 1,eq 95.332 kPa, the first desorption equilibrium pressure P 1,eq Corresponding mole number n of active carbon adsorption nitrogen 1,de The method comprises the following steps:
D. equilibrium pressure P at the first desorption point of isothermal desorption line 1,eq The molar number n of the nitrogen still absorbed by the activated carbon is 95.332 kPa 1,de 1.94X10 -3 mol。
(2) Determining a second desorption data point of the isothermal desorption line
A. Closing the sample tube sealing valve, opening the air extraction three-way valve to switch to an air flow closing state, opening the air extraction quantitative pulse valve to extract air from the reference cavity, and obtaining the pressure P in the reference cavity 2,out Adjusted to 90 kPa, the vacuum pump is controlled by a pumping quantitative pulse valve from a reference cavity V with the volume of 119.6 mL r When the gas is pumped out, the pumping quantitative pulse valve needs to be opened and closed for x times, and the calculation process is as follows:
B. the operating frequency of the bleed pulse valve is 10 Hz, and it takes 142+.10=14.2 seconds to complete the bleed. Closing the air extraction quantitative pulse valve, measuring pressure after 10 seconds, and measuring the value P 2,out 90.004 kPa;
C. the sample tube sealing valve is opened, and the pressure is measured after 10 seconds, and the value P of the pressure is measured 2,eq 91.132 kPa, the second desorption equilibrium pressure P 2,eq Corresponding mole number n of active carbon adsorption nitrogen 2,de The method comprises the following steps:
D. equilibrium pressure P at the second desorption point of isothermal desorption line 2,eq The molar number n of the nitrogen still absorbed by the activated carbon is 91.132 kPa 2,de 1.81X 10 -3 mol。
(3) Determination of isothermal desorption line ith desorption data point
Each time the reference cavity is pumped down by 5 kPa lower than the last balance pressure, when the balance pressure is lower than the absolute pressure by 25 kPa, the pressure difference between the inside and the outside of the pumping quantitative pulse valve is too small, and the time required for pumping by using the pumping quantitative pulse valve is increasedThe air leakage of the sample cavity and the reference cavity is increased, and at the moment, the air suction three-way valve is required to be closed to be switched to an air flow through state for air suction. Setting the pressure P at the i-1 st time of balance i-1,eq 19.776 kPa, corresponding adsorption quantity n i-1,de 1.29×10 -3 mol。
A. Closing the sealing valve of the sample tube, switching the air extraction three-way valve to an air flow through state to extract air from the reference cavity, opening the air extraction three-way valve to an air flow closing state to stop air extraction when the pressure value of the air pressure sensor reaches 15 kPa, and measuring the pressure after 10 seconds, wherein the value P of the pressure is the value P i,out 14.455 kPa;
B. the sample tube sealing valve is opened, and the pressure is measured after 10 seconds, and the value P of the pressure is measured i,eq 15.719 kPa (i-th desorption equilibrium pressure P) i,eq Corresponding mole number n of active carbon adsorption nitrogen i,de The method comprises the following steps:
C. equilibrium pressure P of i-th desorption data point of isothermal desorption line i,eq The molar number n of the nitrogen adsorbed by the activated carbon is 15.719 kPa i,de Is 1.11 multiplied by 10 -3 mol。
And repeating the pumping measurement calculation step until the pressure sensor detects that the pressure reaches below 0.001. 0.001 Pa absolute pressure, stopping the desorption process, and drawing an isothermal desorption line of the active carbon for desorbing nitrogen according to the measurement result.
The following points need to be described:
(1) The drawings of the embodiments of the present invention relate only to the structures related to the embodiments of the present invention, and other structures may refer to the general designs.
(2) In the drawings for describing embodiments of the present invention, the thickness of layers or regions is exaggerated or reduced for clarity, i.e., the drawings are not drawn to actual scale. It will be understood that when an element such as a layer, film, region or substrate is referred to as being "on" or "under" another element, it can be "directly on" or "under" the other element or intervening elements may be present.
(3) The embodiments of the invention and the features of the embodiments can be combined with each other to give new embodiments without conflict.
The present invention is not limited to the above embodiments, but the scope of the invention is defined by the claims.
Claims (8)
1. The integrated module is characterized by comprising a main body module, a sample tube module, a pressure measurement module, a gas path sealing module and a valve module, wherein the pressure measurement module is arranged on the upper surface of the main body module, the sample tube module is arranged on the lower surface of the main body module, the gas path sealing module ensures the sealing of the whole integrated module, and the valve module is arranged on the upper surface and the front surface of the main body module;
the main body module is cuboid, and an air exhaust pipeline interface is arranged on the left side surface of the main body module and used for being connected with a vacuum pump regulating valve; an external air source air inlet hole is formed in the right side surface of the main body module and is used for being connected with an external air source clamping sleeve connector, and a reference cavity cover plate placing groove is formed in the lower portion of the external air source air inlet hole and is used for placing a reference cavity cover plate; the middle part of the upper surface of the main body module is provided with an air pressure sensor sealing ring placing groove for connecting an air pressure sensor, the left side of the air pressure sensor sealing ring placing groove is provided with an air suction three-way valve straight-through air outlet hole, an air suction three-way valve pulsation air outlet hole and an air suction three-way valve air inlet hole for correspondingly accessing the air suction three-way valve, the right side of the air pressure sensor sealing ring placing groove is provided with a sample tube sealing valve air outlet hole and a sample tube sealing valve air inlet hole for correspondingly accessing the sample tube sealing valve, and the right side of the sample tube sealing valve air outlet hole and the sample tube sealing valve air inlet hole is provided with an air charging sealing valve air outlet hole and an air charging sealing valve air inlet hole for correspondingly accessing the air charging sealing valve; the lower surface of the main body module is provided with a sample tube interface mounting groove for mounting the sample tube module; the left side of the front surface of the main body module is provided with an air outlet hole of the air extraction quantitative pulse valve and an air inlet hole of the air extraction quantitative pulse valve, which are used for being correspondingly connected with the air extraction quantitative pulse valve, and the right side of the front surface of the main body module is provided with an air outlet hole of the air inflation quantitative pulse valve and an air inlet hole of the air inflation quantitative pulse valve, which are used for being correspondingly connected with the air inflation quantitative pulse valve.
2. The integrated module for precisely controlling the adsorption and desorption of the gas by pulsation according to claim 1, wherein the air exhaust pipeline connector is provided with a vacuum pump air exhaust coarse pore canal and a vacuum pump air exhaust fine pore canal horizontally and concentrically in sequence in the main body module, the external air source air inlet hole is provided with an external air source air inlet coarse pore canal and an external air source air inlet fine pore canal horizontally and concentrically in sequence in the main body module, the center of the reference cavity cover plate placing groove is provided with a reference cavity sealing ring placing groove and a reference cavity main pore canal opening which is concentric and has a diameter smaller than that of the reference cavity sealing ring placing groove, and the reference cavity main pore canal opening is provided with a reference cavity main pore canal horizontally in the main body module;
the through air outlet of the air suction three-way valve is vertically and downwards provided with an air suction three-way valve through air outlet channel which is communicated with the vacuum pump air suction fine channel; the air pumping three-way valve pulsation air outlet hole is vertically and downwards provided with an air pumping three-way valve pulsation air outlet hole, and the air pumping three-way valve pulsation air outlet hole is communicated with the air pumping quantitative pulse valve air inlet hole; an air inlet channel of the air extraction three-way valve is vertically and downwards opened and communicated with a main channel of the reference cavity;
The air pressure sensor seal ring placing groove is vertically and downwards provided with an air pressure sensor core seat with the concentric diameter smaller than that of the air pressure sensor seal ring placing groove, the air pressure sensor core seat is vertically and downwards provided with an air pressure sensor pore canal, and the air pressure sensor pore canal and the reference cavity main pore canal are intersected at an air pressure sensor pore canal communicating port;
the air outlet hole of the sample tube sealing valve is vertically and downwards provided with a sample tube sealing valve air outlet channel communicated with the sample tube connecting channel, and the air inlet hole of the sample tube sealing valve is vertically and downwards provided with a sample tube sealing valve air inlet channel communicated with the main channel of the reference cavity;
the air outlet hole of the air charging sealing valve is vertically and downwards provided with an air outlet hole channel of the air charging sealing valve which is communicated with the main hole channel of the reference cavity, and the air inlet hole of the air charging sealing valve is vertically and downwards provided with an air inlet hole channel of the air charging sealing valve which is communicated with an air inlet fine hole channel of an external air source;
the air outlet hole of the air charging quantitative pulse valve is horizontally and backwardly provided with an air charging quantitative pulse valve air outlet channel communicated with an air inlet thin channel of an external air source, a non-through air charging quantitative pulse valve expansion hole is horizontally and backwardly arranged between the air outlet hole of the air charging quantitative pulse valve and the air inlet hole of the air charging quantitative pulse valve, and the air inlet hole of the air charging quantitative pulse valve is horizontally and backwardly provided with an air charging quantitative pulse valve air inlet channel communicated with an air inlet thick channel of the external air source;
The air outlet hole of the air extraction quantitative pulse valve is horizontally and backwardly provided with an air outlet hole channel of the air extraction quantitative pulse valve, which is communicated with the air extraction fine hole channel of the vacuum pump, and the air outlet hole of the air extraction quantitative pulse valve and the air inlet hole of the air extraction quantitative pulse valve are horizontally and backwardly provided with a non-through air extraction quantitative pulse valve expansion hole, and the air inlet hole of the air extraction quantitative pulse valve is horizontally and backwardly provided with an air inlet hole channel of the air extraction quantitative pulse valve, which is communicated with the air outlet hole channel of the air extraction three-way valve;
the sample tube interface mounting groove is vertically upwards provided with a sample tube interface fixing platform, and the sample tube interface fixing platform is vertically and concentrically upwards provided with a sample tube connecting pore canal.
3. The integrated module for precisely controlling gas adsorption and desorption by pulsation according to claim 1, wherein the whole body formed by the through air outlet hole of the air extraction three-way valve, the pulsation air outlet hole of the air extraction three-way valve and the air inlet hole of the air extraction three-way valve is symmetrically provided with an air extraction three-way valve fixing threaded hole and an air extraction three-way valve positioning pin hole at both sides, the air extraction three-way valve is positioned on the upper surface of the main body module through the air extraction three-way valve positioning pin hole, forms a seal with the upper surface of the main body module through the air extraction three-way valve sealing ring, and is fixed on the upper surface of the main body module through the air extraction three-way valve fixing threaded hole;
The sample tube sealing valve is positioned on the upper surface of the main body module through the sample tube sealing valve positioning pin hole, forms a seal with the upper surface of the main body module through a sealing valve sealing gasket, and is fixed on the upper surface of the main body module through the sample tube sealing valve fixing threaded hole;
the air inlet and the air outlet of the air sealing valve are symmetrically provided with an air sealing valve fixing threaded hole and an air sealing valve positioning pin hole on two sides of the whole body formed by the air outlet of the air sealing valve and the air inlet of the air sealing valve, the air sealing valve is positioned on the upper surface of the main body module through the air sealing valve positioning pin hole, forms a seal with the upper surface of the main body module through the air sealing valve sealing gasket, and is fixed on the upper surface of the main body module through the air sealing valve fixing threaded hole;
the air outlet hole of the air charging quantitative pulse valve and the air inlet hole of the air charging quantitative pulse valve are symmetrically provided with an air charging quantitative pulse valve fixing threaded hole and an air charging quantitative pulse valve positioning pin hole on both sides of the whole body, the air charging quantitative pulse valve is positioned on the front surface of the main body module through the air charging quantitative pulse valve positioning pin hole, forms a seal with the front surface of the main body module through the air charging quantitative pulse valve sealing gasket, and is fixed on the front surface of the main body module through the air charging quantitative pulse valve fixing threaded hole;
The air outlet hole of the air extraction quantitative pulse valve and the air inlet hole of the air extraction quantitative pulse valve are symmetrically provided with an air extraction quantitative pulse valve fixing threaded hole and an air extraction quantitative pulse valve positioning pin hole on two sides of the whole body, the air extraction quantitative pulse valve is positioned on the front surface of the main body module through an air extraction quantitative pulse valve positioning pin, forms a seal with the front surface of the main body module through an air extraction quantitative pulse valve sealing gasket, and is fixed on the front surface of the main body module through the air extraction quantitative pulse valve fixing threaded hole;
sample tube fixing threaded holes are symmetrically formed in the periphery of the sample tube interface mounting groove, and the sample tube module is fixed to the lower surface of the main body module through the sample tube fixing threaded holes.
4. The integrated module for pulsed accurate control of gas adsorption and desorption according to claim 1, wherein the sample tube module comprises a sample tube, a sample tube lock nut combined sealing ring, a sample tube lock nut O-ring, a sample tube interface, and a sample tube interface O-ring,
the sample tube locking nut is provided with a sample tube locking nut center hole in the center, the upper surface of the sample tube locking nut is provided with a sample tube locking nut platform, a sample tube locking nut combined sealing ring and a sample tube locking nut O-shaped ring are placed on the sample tube locking nut platform from bottom to top and are installed inside a sample tube connector, the center of the sample tube connector is provided with a sample tube connector center hole, the surface of the sample tube connector is symmetrically provided with a sample tube connector through hole, the center of the upper surface of the sample tube connector is provided with a sample tube connector O-shaped ring placing groove, the sample tube connector O-shaped ring placing groove is internally provided with a sample tube connector O-shaped ring, the sample tube connector is fixed on the lower surface of the main body module through a sample tube fixing threaded hole and the sample tube connector through the sample tube locking nut, the sample tube locking nut combined sealing ring and the sample tube locking nut O-shaped ring, and the sample tube locking nut O-shaped ring are fastened through threads, so that the sample tube locking nut O-shaped ring is fastened to expand and compress the sample tube in the radial direction;
The enclosed volume surrounded by the air outlet hole of the sample tube sealing valve, the connecting pore canal of the sample tube, the air outlet pore canal of the sample tube sealing valve and the sample tube on the main body module is called a sample cavity;
the enclosed volume surrounded by the air suction three-way valve air inlet, the air pressure sensor sealing ring placing groove, the sample tube sealing valve air inlet, the air inflation sealing valve air outlet and the reference cavity cover plate is called a reference cavity.
5. The integrated module for pulsating precise control of gas adsorption and desorption according to claim 1, wherein the gas path sealing module comprises a vacuum pump regulating valve, a vacuum pump combination sealing ring, an external gas source clamping sleeve joint, an external gas source combination sealing ring, a reference cavity sealing O-ring and a reference cavity cover plate,
the reference cavity sealing O-shaped ring is arranged in the reference cavity sealing ring placing groove, an end face seal is formed by compressing the reference cavity cover plate, an inflatable filter is arranged at the joint of the external air source air inlet coarse pore canal and the external air source air inlet fine pore canal, an external air source clamping sleeve joint is fixed on the right side surface of the main body module through threads in an external air source air inlet hole, the external air source combined sealing ring is compressed to form a seal, and the inflatable filter is compressed through the external air source combined sealing ring;
The vacuum pump regulating valve is fixed on the left side surface of the main body module through threads in the air extraction pipeline interface, and compresses the vacuum pump combined sealing ring to form a seal;
four reference cavity cover plate through holes are symmetrically formed in the periphery of the reference cavity cover plate, reference cavity cover plate fixing threaded holes are symmetrically formed in the periphery of the reference cavity cover plate placing groove, fastening screws are screwed into the reference cavity cover plate fixing threaded holes through the four reference cavity cover plate through holes to be fixed on the right side surface of the main body module, and reference cavity sealing O-shaped rings are placed in the reference cavity sealing ring placing groove.
6. The integrated module for precisely controlling the adsorption and desorption of gas by pulsation according to claim 1, wherein the valve module comprises an air extraction three-way valve, an air extraction three-way valve sealing ring, a sample tube sealing valve gasket, an air inflation sealing valve gasket, an air inflation quantitative pulse valve gasket, an air extraction quantitative pulse valve and an air extraction quantitative pulse valve gasket, and the valves of the valve module are all seat-mounted electromagnetic valves and are sealed with a smooth plane through the gaskets;
the lower surface of the air extraction three-way valve is horizontally provided with an air extraction three-way valve fixing through hole, an air extraction three-way valve through air outlet, an air extraction three-way valve pulsation air outlet, an air extraction three-way valve air inlet and an air extraction three-way valve positioning pin, the lower surface of the air extraction three-way valve is provided with an air extraction three-way valve sealing groove, and an air extraction three-way valve sealing gasket is placed in the air extraction three-way valve sealing groove; when the air extraction three-way valve is in a closed state, the air inlet of the air extraction three-way valve is communicated with the through air outlet of the air extraction three-way valve, and the air inlet of the air extraction three-way valve is blocked with the pulsating air outlet of the air extraction three-way valve; when the air extraction three-way valve is in an open state, the air inlet of the air extraction three-way valve is blocked from the through air outlet of the air extraction three-way valve, and the air inlet of the air extraction three-way valve is communicated with the pulsating air outlet of the air extraction three-way valve;
The lower surface center of the air extraction quantitative pulse valve is symmetrically provided with an air extraction quantitative pulse valve fixing through hole and an air extraction quantitative pulse valve positioning pin, the center of the lower surface of the air extraction quantitative pulse valve is provided with an air extraction quantitative pulse valve expansion port, two sides of the air extraction quantitative pulse valve expansion port are symmetrically provided with an air extraction quantitative pulse valve air inlet and an air extraction quantitative pulse valve air outlet, the lower surface of the air extraction quantitative pulse valve is provided with an air extraction quantitative pulse valve sealing groove, and an air extraction quantitative pulse valve sealing gasket is placed in the air extraction quantitative pulse valve sealing groove; when the air extraction quantitative pulse valve is in an open state, the air inlet of the air extraction quantitative pulse valve and the air outlet of the air extraction quantitative pulse valve are alternately opened and closed at the frequency of 10Hz, the air between the air inlet of the air extraction quantitative pulse valve and the air outlet of the air extraction quantitative pulse valve is discharged, and when the air extraction quantitative pulse valve is in a closed state, the air inlet of the air extraction quantitative pulse valve is kept sealed to block the air;
the center of the lower surface of the sample tube sealing valve is symmetrically provided with a sample tube sealing valve fixing through hole and a sample tube sealing valve positioning pin, the center of the lower surface of the sample tube sealing valve is provided with a sample tube sealing valve air inlet, the side of the sample tube sealing valve air inlet is provided with a sample tube sealing valve air outlet, the lower surface of the sample tube sealing valve is provided with a sample tube sealing valve sealing groove, and a sample tube sealing gasket is placed in the sample tube sealing valve sealing groove; when the sample tube sealing valve is in an open state, an air inlet of the sample tube sealing valve is communicated with an air outlet of the sample tube sealing valve; when the sample tube sealing valve is in a closed state, the air inlet of the sample tube sealing valve is blocked from the air outlet of the sample tube sealing valve;
The center of the lower surface of the quantitative inflation pulse valve is symmetrically provided with two quantitative inflation pulse valve fixing through holes and quantitative inflation pulse valve positioning pins, the center of the lower surface of the quantitative inflation pulse valve is provided with quantitative inflation pulse valve expansion openings, two sides of each quantitative inflation pulse valve expansion opening are symmetrically provided with quantitative inflation pulse valve air outlets and quantitative inflation pulse valve air inlets, and are provided with quantitative inflation pulse valve sealing grooves, and quantitative inflation pulse valve sealing gaskets are placed in the quantitative inflation pulse valve sealing grooves; when the quantitative inflation pulse valve is in an open state, the air inlet of the quantitative inflation pulse valve and the air outlet of the quantitative inflation pulse valve are alternately opened and closed at the frequency of 10Hz, and the air between the air inlet of the quantitative inflation pulse valve and the air outlet of the quantitative inflation pulse valve is discharged; when the quantitative inflation pulse valve is in a closed state, the air inlet of the quantitative inflation pulse valve is kept sealed to block the air;
the center of the lower surface of the inflatable sealing valve is symmetrically provided with two inflatable sealing valve fixing through holes and an inflatable sealing valve positioning pin, the center of the lower surface of the inflatable sealing valve is provided with an inflatable sealing valve air outlet, the side of the inflatable sealing valve air outlet is provided with an inflatable sealing valve air inlet, the lower surface of the inflatable sealing valve is provided with an inflatable sealing valve sealing groove, and an inflatable sealing valve sealing gasket is placed in the inflatable sealing valve sealing groove; when the air charging sealing valve is in an open state, an air inlet of the air charging sealing valve is communicated with an air outlet of the air charging sealing valve; when the air charging sealing valve is in a closed state, the air inlet of the air charging sealing valve is blocked from the air outlet of the air charging sealing valve.
7. The integrated module for precisely controlling gas adsorption and desorption according to claim 6, wherein a three-way valve positioning pin on the three-way valve is aligned with a three-way valve positioning pin hole on the main body module, a three-way valve through air outlet on the three-way valve is communicated with a three-way valve through air outlet on the main body module, a three-way valve pulsation air outlet on the three-way valve is communicated with a three-way valve pulsation air outlet on the main body module, a three-way valve air inlet on the three-way valve is communicated with a three-way valve air inlet on the main body module, a fastening screw is screwed into a three-way valve fixing threaded hole on the main body module through a three-way valve fixing through hole on the three-way valve, and after the fastening screw is screwed, the three-way valve forms a seal with the main body module;
the air inlet of the air quantitative pulse valve on the air quantitative pulse valve is communicated with the air inlet of the air quantitative pulse valve on the main body module, the fastening screw is screwed into the air quantitative pulse valve fixing threaded hole on the main body module through the air quantitative pulse valve fixing through hole on the air quantitative pulse valve, and after the fastening screw is screwed up, the air quantitative pulse valve and the main body module form a seal;
The air suction quantitative pulse valve positioning pin on the air suction quantitative pulse valve is aligned with the air suction quantitative pulse valve positioning pin hole on the main body module, the air suction quantitative pulse valve air inlet on the air suction quantitative pulse valve is communicated with the air suction quantitative pulse valve air inlet on the main body module, the air suction quantitative pulse valve expansion port on the air suction quantitative pulse valve is communicated with the air suction quantitative pulse valve expansion hole on the main body module, the air outlet of the air suction quantitative pulse valve on the air suction quantitative pulse valve is communicated with the air outlet of the air suction quantitative pulse valve on the main body module, the fastening screw is screwed into the air suction quantitative pulse valve fixing threaded hole on the main body module through the air suction quantitative pulse valve fixing through hole on the air suction quantitative pulse valve, and after the fastening screw is screwed up, the air suction quantitative pulse valve and the main body module form a seal;
the sample tube sealing valve positioning pin on the sample tube sealing valve is aligned with the sample tube sealing valve positioning pin hole on the main body module, the sample tube sealing valve air inlet on the sample tube sealing valve is communicated with the sample tube sealing valve air inlet on the main body module, the sample tube sealing valve air outlet on the sample tube sealing valve is communicated with the sample tube sealing valve air outlet on the main body module, the fastening screw is screwed into the sample tube sealing valve fixing threaded hole on the main body module through the sample tube sealing valve fixing through hole on the sample tube sealing valve, and after the fastening screw is screwed, the sample tube sealing valve and the main body module form sealing;
The air-filled sealing valve positioning pin on the air-filled sealing valve is aligned with the air-filled sealing valve positioning pin hole on the main body module, the air inlet of the air-filled sealing valve on the air-filled sealing valve is communicated with the air inlet of the air-filled sealing valve on the main body module, the air outlet of the air-filled sealing valve on the air-filled sealing valve is communicated with the air outlet of the air-filled sealing valve on the main body module, the fastening screw is screwed into the air-filled sealing valve fixing threaded hole on the main body module through the air-filled sealing valve fixing through hole on the air-filled sealing valve, and after the fastening screw is screwed, the air-filled sealing valve and the main body module form sealing.
8. A control method of an integrated module for controlling gas adsorption and desorption based on pulsation accuracy according to any one of claims 1 to 7, comprising the steps of:
s1, filling an adsorbent: unscrewing a sample tube locking nut, taking down the sample tube, weighing the mass of the sample tube, loading the adsorbent to be tested, weighing the total mass of the sample tube and the adsorbent, inserting the sample tube into a sample tube interface, screwing the sample tube locking nut to finish the filling of the adsorbent, placing the sample tube containing the adsorbent into a liquid adsorbent, and closing all valves;
s2, cleaning the reference cavity and the sample cavity: switching an external air source to high-purity argon, opening an external vacuum pump, adjusting a vacuum pump adjusting valve, closing an air extraction three-way valve, switching to an air flow straight-through state, vacuumizing a reference cavity, opening a sample tube sealing valve to vacuumize the sample cavity after 10 seconds, switching the air extraction three-way valve to an air flow closing state to stop air extraction when the pressure reaches below 0.001 Pa after the reference cavity and the gas in the sample cavity pass through a sample tube connecting pore channel, a sample tube sealing valve air outlet pore channel, a sample tube sealing valve air inlet pore channel, a reference cavity main pore channel, an air extraction three-way valve air inlet pore channel, an air extraction three-way valve straight-through air outlet pore channel, a vacuum pump air exhaust fine pore channel, a vacuum pump air exhaust coarse pore channel and a vacuum pump adjusting valve are arranged, opening an inflation sealing valve, filling argon into a reference cavity and a sample cavity, enabling the argon to enter a main body module through an external air source clamping sleeve joint, enabling the argon to enter an external air source air inlet thin pore channel through an external air source air inlet thick pore channel and an inflation filter piece, enabling an inflation sealing valve air inlet pore channel and an inflation sealing valve air outlet pore channel to enter a reference cavity main pore channel, enabling part of the argon in the reference cavity main pore channel to enter a core seat of a pneumatic sensor, enabling the other part of the argon to enter a sample tube sealing valve air inlet pore channel, a sample tube sealing valve and a sample tube sealing valve air outlet pore channel, enabling the argon to enter a sample tube through a sample tube connecting pore channel, closing the inflation sealing valve when the pressure value measured by the pneumatic sensor reaches 27-30 kPa, and closing the sample tube sealing valve after 10 seconds, so as to finish one-time cleaning;
S3, air volume calibration: repeating the step S2 four times to finish the replacement cleaning of the reference cavity and the sample cavity; switching the air suction three-way valve to an air flow through state, vacuumizing the reference cavity, opening the sample tube sealing valve to vacuumize the sample cavity after 10 seconds, measuring and recording the pressure at the moment by the air pressure sensor after 10 seconds when the pressure reaches below 0.001 Pa, opening the air suction three-way valve to an air flow closing state, measuring and recording the pressure at the moment by the air pressure sensor, opening an inflatable sealing valve to charge argon into a reference cavity, enabling the argon to enter a main body module through an external air source clamping sleeve joint, enabling an external air source air inlet rough pore channel, an inflatable filter piece, an external air source air inlet fine pore channel, an inflatable sealing valve air inlet pore channel, an inflatable sealing valve and an inflatable sealing valve air outlet pore channel to enter a reference cavity main pore channel, enabling part of the argon in the reference cavity main pore channel to enter a pressure sensor core seat, enabling the other part of the argon to enter a sample tube sealing valve air inlet pore channel, closing the inflatable sealing valve when the pressure sensor detects that the pressure is 27-30 kPa, measuring and recording the pressure value at the moment after 10 seconds, opening the sample tube sealing valve, enabling the argon to enter a sample tube through the sample tube sealing valve, the sample tube sealing valve air outlet pore channel and the sample tube connecting pore channel, and monitoring the gas pressure in real time by the pressure sensor, and measuring and recording the pressure value at the moment after 10 seconds;
S4, measuring adsorption data points at low pressure: closing a sample tube sealing valve, starting a vacuum pump, closing an air extraction three-way valve, switching to an air flow through state, vacuumizing a reference cavity, opening the sample tube sealing valve after 10 seconds, vacuumizing the sample cavity, enabling argon in the reference cavity and the sample cavity to directly pass through an air inlet channel of the air extraction three-way valve, an air outlet channel of the air extraction three-way valve, an air pumping fine channel of the vacuum pump, a coarse channel of the vacuum pump and a regulating valve of the vacuum pump, measuring gas pressure by a pressure sensor, opening the air extraction three-way valve to a gas flow closing state when the pressure reaches below 0.001 Pa, measuring the pressure at the moment after 10 seconds, closing the sample tube sealing valve, connecting an external air source clamping sleeve joint with a high-purity adsorbate gas cylinder, opening the air filling sealing valve into the reference cavity, enabling adsorbate to enter a main module through the external air source clamping sleeve joint, enabling the external air inlet coarse channel, the air inlet fine channel of the air source, the air inlet sealing valve and the air inlet fine channel of the air filling sealing valve to enter the main channel of the reference cavity, enabling part of the adsorbate to enter a core seat of the air pressure sensor when the pressure of the pressure sensor to be divided into two flow directions, and when the pressure of the adsorption mass enters the core seat of the air pressure sensor is measured, and the pressure of the pressure sensor is measured after 10 seconds, and the pressure of the sample tube is measured after 10 seconds is recorded, and the pressure is measured;
S5, measuring adsorption data points at high pressure: when the pressure sensor monitors that the pressure in the main pore canal of the reference cavity is higher than 25 kPa, the time required for air intake of the air-filled filter piece is increased, so that the air leakage of the sample cavity and the reference cavity is increased, at the moment, the air intake of the air-filled quantitative pulse valve is switched to, the adsorbate enters the main module through an external air source clamping sleeve joint, and enters the main module through an external air source air intake rough pore canal, an air-filled quantitative pulse valve air intake pore canal, an air-filled quantitative pulse valve air outlet pore canal, an external air source air intake fine pore canal, an air-filled sealing valve air intake pore canal, an air-filled sealing valve air-outlet pore canal and an air-filled sealing valve air-outlet pore canal enter the main pore canal of the reference cavity, wherein the adsorbate in the main pore canal of the reference cavity is divided into two flow directions, one part of adsorbate enters the air-pressure sensor core seat, the other part of adsorbate enters the air-inlet pore canal of the sample tube sealing valve, the air-filled sealing valve is closed, the air pressure value is measured and recorded after 10 seconds, the sample tube sealing valve is opened, and the air pressure value is measured and recorded at the moment after 10 seconds;
s6, repeating the step S5 until the air pressure sensor detects that the pressure in the reference cavity reaches a standard atmospheric pressure, stopping measuring adsorption data, and drawing an isothermal adsorption line according to a measurement result;
S7, determination of desorption data points at high pressure: measuring isothermal desorption lines by taking the state at the end of the adsorption process as an initial state, closing all valves, and placing a sample tube containing the adsorbent in a temperature environment where the adsorbent is still positioned in the adsorption process, wherein the absolute pressure at the interface of an air extraction pipeline is close to 0 kPa; at the moment, the pressure difference at the interface of the pressure in the reference cavity and the air extraction pipeline is too large, the pressure in the reference cavity can be changed too fast through direct air extraction, and the air extraction three-way valve is not fed back timely due to measurement lag of the air pressure sensor, so that the air extraction quantitative pulse valve is adopted for air extraction; switching the air extraction three-way valve to an air flow closing state, opening the air extraction quantitative pulse valve to extract air from the reference cavity, opening the air extraction quantitative pulse valve to extract the air from the reference cavity main pore canal, and measuring and recording the air pressure value at the moment after 10 seconds, opening the sample tube sealing valve, and measuring and recording the pressure value at the moment after 10 seconds;
S8, measuring desorption data points at low pressure: when the balance pressure is lower than the absolute pressure of 25 kPa, the pressure difference between the inside and the outside of the air extraction quantitative pulse valve is too small, the time required for air extraction by using the air extraction quantitative pulse valve is increased, so that the air leakage of the sample cavity and the reference cavity is increased, and at the moment, the air extraction three-way valve is required to be closed to be switched to an air flow through state for air extraction; closing a sample tube sealing valve, switching the air extraction three-way valve to an air flow through state to extract air from a reference cavity, discharging the air in a main pore canal of the reference cavity through an air inlet pore canal of the air extraction three-way valve, a direct air outlet pore canal of the air extraction three-way valve, a vacuum pump air suction fine pore canal, a vacuum pump air suction coarse pore canal and a vacuum pump regulating valve, opening the air extraction three-way valve to an air flow closing state to stop air extraction when the pressure value detected by an air pressure sensor reaches a preset pressure of +/-1 kPa, measuring and recording the pressure after 10 seconds, opening the sample tube sealing valve, and measuring and recording the pressure after 10 seconds;
s9, repeating the steps S7 and S8 until the pressure sensor detects that the pressure reaches below 0.001 and Pa absolute pressure, stopping measuring desorption data, and drawing an isothermal desorption line at the temperature according to the measurement result;
S10, residual gas treatment: and opening the sealing valve of the sample tube, closing the air extraction three-way valve, switching the air extraction three-way valve to an air flow through state, and discharging air in the sample cavity and the reference cavity through the air inlet pore canal of the air extraction three-way valve, the air outlet pore canal of the air extraction three-way valve, the air pumping fine pore canal of the vacuum pump, the air pumping coarse pore canal of the vacuum pump and the regulating valve of the vacuum pump, wherein the air pressure sensor measures the air pressure, and when the pressure is less than 0.001 Pa, opening the air extraction three-way valve, switching the air extraction three-way valve to an air flow closing state, and stopping air extraction.
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