CN117433970A - System and method for testing chemical vapor barrier properties of barrier materials - Google Patents
System and method for testing chemical vapor barrier properties of barrier materials Download PDFInfo
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- 238000012360 testing method Methods 0.000 title claims abstract description 284
- 239000000126 substance Substances 0.000 title claims abstract description 97
- 239000000463 material Substances 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 30
- 230000004888 barrier function Effects 0.000 title claims description 21
- 238000001819 mass spectrum Methods 0.000 claims abstract description 32
- 238000012546 transfer Methods 0.000 claims description 71
- 238000002347 injection Methods 0.000 claims description 43
- 239000007924 injection Substances 0.000 claims description 43
- 230000007246 mechanism Effects 0.000 claims description 30
- 238000007789 sealing Methods 0.000 claims description 19
- 238000005259 measurement Methods 0.000 claims description 18
- 230000008859 change Effects 0.000 claims description 15
- 238000004891 communication Methods 0.000 claims description 9
- 238000006073 displacement reaction Methods 0.000 claims description 9
- 238000007599 discharging Methods 0.000 claims description 4
- 231100000331 toxic Toxicity 0.000 claims description 3
- 230000002588 toxic effect Effects 0.000 claims description 3
- 230000000149 penetrating effect Effects 0.000 claims 1
- 230000001681 protective effect Effects 0.000 abstract description 21
- 239000007789 gas Substances 0.000 description 155
- 238000005070 sampling Methods 0.000 description 8
- 238000004949 mass spectrometry Methods 0.000 description 7
- 238000010998 test method Methods 0.000 description 7
- 238000010586 diagram Methods 0.000 description 6
- JOZDADPMWLVEJK-UHFFFAOYSA-N 1-pentylsulfanylpentane Chemical compound CCCCCSCCCCC JOZDADPMWLVEJK-UHFFFAOYSA-N 0.000 description 5
- ZERULLAPCVRMCO-UHFFFAOYSA-N Dipropyl sulfide Chemical compound CCCSCCC ZERULLAPCVRMCO-UHFFFAOYSA-N 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 4
- 239000004973 liquid crystal related substance Substances 0.000 description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 230000001143 conditioned effect Effects 0.000 description 3
- VONWDASPFIQPDY-UHFFFAOYSA-N dimethyl methylphosphonate Chemical compound COP(C)(=O)OC VONWDASPFIQPDY-UHFFFAOYSA-N 0.000 description 3
- 239000012466 permeate Substances 0.000 description 3
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 230000013011 mating Effects 0.000 description 2
- 230000035515 penetration Effects 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 239000001294 propane Substances 0.000 description 2
- 238000009423 ventilation Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000003750 conditioning effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 239000000383 hazardous chemical Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000010619 multiway switching Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 231100000167 toxic agent Toxicity 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
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- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Testing Resistance To Weather, Investigating Materials By Mechanical Methods (AREA)
Abstract
The invention discloses a system and a method for testing chemical vapor protection performance of a protection material, wherein the system comprises a vapor generation device, a test clamping device and an online mass spectrum device; the steam generating device is used for generating test gas containing chemical steam; the test clamping device comprises a first clamping unit and a second clamping unit; the first clamping unit and the second clamping unit are arranged to be capable of clamping a sample to be tested; the first clamping unit is provided with a steam inlet and an exhaust port; the steam inlet is communicated with the steam generating device; the second clamping unit is provided with a steam outlet; the exhaust port is used for exhausting the residual testing gas in the first clamping unit; and the online mass spectrum device is connected with the vapor outlet and is used for quantitatively detecting the permeated test gas. The system and the method have wide application range and high accuracy, and can be suitable for testing the chemical vapor protection performance of the breathable and semi-permeable protective material.
Description
Technical Field
The present invention relates to a system and a method for testing the chemical vapor barrier property of a protective material, and more particularly, to a system and a method for testing the chemical vapor barrier property of a protective material which can be used for semi-ventilation.
Background
In recent years, chemical protective clothing plays an important role in the fields of army and police anti-terrorism, fire rescue and industrial protection. Chemical protective clothing relies on the insulating and absorptive properties of the material to protect personnel from hazardous chemical vapors.
The traditional chemical vapor protection test system and method generally adopt test paper to judge the end point, the method has the problems of inaccurate end point judgment and low test efficiency, in the related standard method for evaluating the protection performance of the inner layer material of the gas suit, congo red-chloramine indicator paper is often used for indicating the change condition of the end point, and the period from the passage of chemical vapor to the blue of the indicator paper is called gas-gas protection time. CN105136508A discloses a DMMP vapor guard dose test system and a test method thereof, the system comprising a DMMP vapor generation chamber, a constant temperature sampling chamber, a central control and product test chamber, and a gas discharge chamber; a test sampling system and a constant temperature device are arranged in the constant temperature sampling chamber. The test system has a complex structure, the system can not measure a plurality of samples at the same time, the system adopts a toxic agent monitor to measure the concentration of the transmitted DMMP vapor, the concentration data of the test process can not be obtained, and the judgment is not accurate enough.
Among the existing systems and methods for testing the protective properties of chemical vapor, there are the above-mentioned convection penetration test methods for breathable materials and also penetration test methods (droplet method) specifically for airtight materials, but for semi-breathable materials, the test systems and methods using both breathable materials and airtight materials are not suitable for evaluating the protective properties thereof.
Disclosure of Invention
Accordingly, an object of the present invention is to provide a system for testing the chemical vapor protection performance of a protective material, which has a wide application range and can be used for testing the protection performance of a breathable and semi-breathable material. Furthermore, the method has the advantages of accurate judgment of the protection end point and high test efficiency. The invention further aims to provide a method for performing chemical vapor protection test by adopting the test system, which has high accuracy and high test efficiency.
The aim of the invention is realized by the following technical scheme.
In a first aspect, the present invention provides a system for testing chemical vapor barrier properties of a barrier material, comprising:
a vapor generation device for generating a test gas containing chemical vapor;
a test clamping device comprising a first clamping unit and a second clamping unit; the first clamping unit and the second clamping unit are stacked, the first clamping unit is located above the second clamping unit, and the first clamping unit and the second clamping unit are arranged to be capable of clamping a sample to be tested; the first clamping unit is provided with a steam inlet and an exhaust port; the steam inlet is communicated with the steam generating device and is used for introducing test gas into the test clamping device; the second clamping unit is provided with a steam outlet; the steam outlet is used for discharging test gas permeated by the test sample; the exhaust port is used for exhausting the residual testing gas in the first clamping unit;
And the online mass spectrum device is connected with the vapor outlet and is used for quantitatively detecting the permeated test gas.
According to the system of the present invention, the system, preferably,
the sample injection switching device is also included;
the steam generating device is provided with a plurality of parallel gas path pipelines for the test gas to circulate; the test clamping devices are arranged in a plurality, and each gas path pipeline is connected with a steam inlet of one test clamping device respectively;
the steam outlet of the test clamping device is connected with the online mass spectrum device through the sample injection switching device; the sample injection switching device is arranged to be capable of switching a plurality of gas paths to be tested, so that only one gas path to be tested is communicated with the online mass spectrum device at the same time.
The system according to the invention preferably:
the steam generating device further comprises a chemical steam generator, a humidity generator, a mixer, a plurality of flow meters and a plurality of one-way valves; wherein,
the chemical vapor generator is used for generating toxic air containing chemical vapor;
the humidity generator is used for generating air after humidity adjustment;
the mixer is respectively connected with the chemical vapor generator and the humidity generator and is used for generating test gas containing chemical vapor;
The gas path pipeline is connected with the mixer; each gas path pipeline is provided with a flowmeter and a one-way valve respectively; the flowmeter is used for controlling the flow rate of the test gas, and the one-way valve is used for controlling the flow direction of the test gas.
According to the system of the invention, preferably, the sample injection switching device is provided with a plurality of test gas path inlets and a gas path outlet; the gas path outlet is connected with an online mass spectrum device; the plurality of test gas path inlets are respectively communicated with the plurality of steam outlets; a plurality of air paths to be tested can be correspondingly formed between a plurality of test air path inlets and one air path outlet.
Preferably, the system according to the present invention, the test fixture further comprises a sealing unit and a locking unit,
the first clamping unit is further provided with a first cavity and a first annular groove; the steam inlet is positioned at the top of the first clamping unit and is communicated with the first cavity; the first annular groove is arranged around the first cavity and is not communicated with the first cavity; the exhaust port is communicated with the first cavity; the first annular groove is arranged to contain a heat transfer medium so that the test gas in the first cavity is maintained at a set temperature;
The second clamping unit is also provided with a second cavity and a second annular groove; the steam outlet is positioned at the bottom of the second clamping unit and is communicated with the second cavity; the second annular groove is arranged around the second cavity and is not communicated with the second cavity; the second annular groove is arranged to contain a heat transfer medium so that the test gas in the second cavity is maintained at a set temperature;
the sealing unit is positioned below the sample to be tested; the sealing unit is arranged to enhance the degree of sealing between the first clamping unit and the second clamping unit;
the locking unit is respectively connected with the first clamping unit and the second clamping unit, and the locking unit is arranged to be capable of fixing the first clamping unit and the second clamping unit.
The system according to the invention preferably:
the first clamping unit is also provided with a first heat transfer medium inlet, a first heat transfer medium outlet and a temperature measuring port; the first heat transfer medium inlet and the first heat transfer medium outlet are respectively communicated with the first annular groove; the temperature measuring port is communicated with the first cavity;
the second clamping unit is also provided with a second heat transfer medium inlet, a second heat transfer medium outlet and a replacement gas inlet; the second heat transfer medium inlet and the second heat transfer medium outlet are respectively communicated with the second annular groove; the displacement gas inlet is in communication with the second cavity.
Preferably, the locking unit comprises a first locking mechanism and a second locking mechanism; the first locking mechanism and the second locking mechanism are oppositely arranged; wherein,
the first locking mechanism comprises a bolt and an engagement piece; the bolts are arranged to penetrate through the connecting piece and are fixed on the first clamping unit and the second clamping unit; the connecting piece is arranged to be foldable;
the second locking mechanism comprises a handle and a lock ring and a lock catch which are matched with each other; the lock catch is arranged on the second clamping unit; the lock ring is connected with a handle, and a part of the handle is arranged on the first clamping unit; the second locking mechanism is configured to lock the shackle with the shackle or to separate the shackle from the shackle by operating the handle.
In a second aspect, the present invention provides a method of chemical vapor protection testing a test sample using a system for testing chemical vapor protection properties of a protective material as described above, comprising the steps of:
step 1, setting corresponding parameters;
step 2, making the test gas containing chemical vapor generated by the vapor generating device reach the required concentration;
Step 3, mounting the sample to be tested in a test clamping device;
step 4, performing protection measurement on the sample to be tested;
and 5, after the measurement is finished, drawing a curve by taking time as an abscissa and taking a vapor concentration value as an ordinate, and obtaining a change curve of vapor permeation concentration along with time.
In a third aspect, the present invention also provides a method for chemical vapor protection testing of a test sample using the system for testing chemical vapor protection properties of a protective material as described above, comprising the steps of:
s1, setting corresponding parameters;
s2, enabling the test gas containing chemical vapor generated by the vapor generating device to reach the required concentration;
s3, respectively installing a plurality of samples to be tested in a plurality of test clamping devices;
s4, performing protection measurement on the sample to be tested;
and S5, after the measurement is finished, drawing a curve by taking time as an abscissa and taking a vapor concentration value as an ordinate, and obtaining a change curve of vapor permeation concentration along with time.
The method according to the invention preferably:
in S1, the parameters include the concentration of chemical vapor in the test gas, the test temperature, and the relative humidity of the test gas;
s3, clamping the sample to be tested between the first clamping unit and the second clamping unit and fixing the test clamping device;
S4, the test gas is respectively introduced into a plurality of test clamping devices from a plurality of gas path pipelines of the vapor generating device, is permeated through each test sample and is respectively discharged from vapor outlets of the plurality of test clamping devices to the sample injection switching device; the sample injection switching device automatically switches the gas paths to be tested at set interval time, so that only one gas path to be tested is communicated with the online mass spectrum device at the same time; the online mass spectrum device records the vapor signal value coming in from the sample injection switching device in real time and converts the vapor signal value into a vapor concentration value;
in S5, after the vapor signal value no longer rises and becomes stable, the test is stopped.
The system for testing the chemical vapor protection performance of the protective material has wide application range, and can be used for testing the protection performance of breathable and semi-breathable materials; moreover, compared with the traditional method for judging the protection end point time by adopting test paper, the system provided by the invention has the advantage that the judgment of the protection end point time is more accurate. Further, simultaneous testing of a plurality of samples to be tested (a plurality of samples to be tested of the same material or a plurality of samples to be tested of different materials) can be achieved, errors are small, and testing efficiency is high. In addition, it can realize the protective performance test at various temperatures. The method for performing chemical vapor protection test by adopting the system has high accuracy and high test efficiency.
Drawings
Fig. 1 is a schematic structural diagram of a system for testing chemical vapor barrier properties of a barrier material according to the present invention.
Fig. 2 is a schematic structural diagram of a test clamping device according to the present invention.
Fig. 3 is a schematic cross-sectional view of a first clamping unit according to the present invention.
Fig. 4 is an exploded view of fig. 2.
Fig. 5 is a schematic diagram of the working principle of a sample injection switching device of the present invention.
FIG. 6 is a graph showing the change in vapor permeation concentration with time in example 2 of the present invention.
FIG. 7 is a graph showing the change in vapor permeation concentration with time in example 3 of the present invention.
The reference numerals are explained as follows:
the device comprises a 1-vapor generating device, a 11-chemical vapor generator, a 12-humidity generator, a 13-mixer, a 14-flowmeter, a 15-one-way valve, a 2-test clamping device, a 21-first clamping unit, a 211-vapor inlet, a 213-first cavity, a 214-first annular groove, a 22-second clamping unit, a 23-sealing unit, a 24-locking unit, a 241-first locking mechanism, a 2411-connector, a 242-second locking mechanism, a 2421-handle, a 2422-locking ring, a 2423-locking buckle, a 101-vapor inlet connector, a 102-exhaust connector, a 103-first heat transfer medium inlet connector, a 104-first heat transfer medium outlet connector, a 105-temperature measuring port connector, a 106-vapor outlet connector, a 107-displacement gas inlet connector, a 108-second heat transfer medium inlet connector, a 109-second heat transfer medium outlet connector, a 3-sample switching device, A-A way, B-way, a-way B, a-way C way inlet, a1-B way inlet, a 3-way inlet, B4-way C inlet, a 2-first exhaust vent, B1-second exhaust vent, a 2-way B, a 2-first exhaust vent, a 2-way vent, a 2-B, and a line connection.
Detailed Description
The system and method of the present invention are described below by way of example only, but the scope of the present invention is not limited thereto.
< System for testing chemical vapor barrier Properties of protective Material >
The system of the present invention is a collection of devices.
In certain embodiments, the system comprises a vapor generating device, a test clamping device, and an online mass spectrometry device, connected in sequence. In this embodiment, the vapor generating device forms only one gas path conduit through which the test gas flows.
In other embodiments, the system includes a vapor generation device, a plurality of test clamping devices, a sample switching device, and an online mass spectrometry device. In this embodiment, the steam generator is formed with a plurality of parallel gas path pipes through which the test gas flows.
The following is a detailed description.
Steam generator
The vapor generating device of the present invention is used for generating a test gas containing chemical vapor. In the present invention, the chemical vapor includes, but is not limited to, vapor formed from toluene, propane sulfide, amyl sulfide, and the like.
The structure of the vapor generating device of the present invention is not particularly limited, and those known in the art can be employed. The steam generating device comprises a chemical steam generator, a humidity generator, a mixer, a flowmeter and a one-way valve. The chemical vapor generator is used for generating contaminated air containing chemical vapor. The humidity generator is used for generating air after humidity conditioning. A toxic solvent capable of forming chemical vapor is placed in the chemical vapor generator. The humidity generator contains water. Compressed air may be introduced into the chemical vapor generator and the humidity generator. The mixer is connected with the chemical vapor generator and the humidity generator respectively and is used for generating test gas containing chemical vapor. The flowmeter is used for controlling the flow rate of the test gas. The check valve is used for controlling the flowing direction of the test gas.
In certain embodiments, the mixer may also be coupled to an on-line mass spectrometry device. This allows quantitative determination of the chemical vapor concentration in the mixer.
In certain embodiments, the vapor generating device has a gas path conduit through which the test gas flows. At this time, the steam generating device comprises a chemical steam generator, a humidity generator, a mixer, a flowmeter and a one-way valve which are arranged on the gas path pipeline. The mixer is connected with the flowmeter and the one-way valve in sequence.
In a preferred embodiment, the vapor generating device forms a plurality of parallel gas path conduits through which the test gas flows. The test gas is distributed in the plurality of gas path pipes to circulate at a set flow rate. This can improve the test efficiency. In this case, the vapor generating device of the present invention includes a chemical vapor generator, a humidity generator, a mixer, a plurality of flow meters, and a plurality of check valves. Each gas pipeline is provided with one flowmeter and one-way valve. The plurality of flowmeters are arranged in parallel. The plurality of check valves are arranged in parallel. One end of each one-way valve is connected with a flowmeter, and the other end of each one-way valve is connected with a steam inlet of a test clamping device. Thus being beneficial to accurate test and improving test efficiency. In one embodiment of the present invention, the number of flow meters is three and the number of check valves is three.
The vapor generating device can be further provided with a liquid crystal touch screen, and parameters such as temperature, humidity, flow, vapor sample injection amount and the like can be set through the liquid crystal touch screen.
Test clamping device
The test clamping device can clamp the test sample to be tested.
In certain embodiments, the test fixture is one. In other embodiments, there are multiple test fixtures, e.g., more than two test fixtures; the number of the plurality of test clamping devices is consistent with the number of the plurality of air channel pipelines.
The test clamping device comprises a first clamping unit, a second clamping unit, a sealing unit and a locking unit. Optionally, a linker unit is also included.
The first clamping unit and the second clamping unit are stacked, the first clamping unit is located above the second clamping unit, and the first clamping unit and the second clamping unit can clamp a sample to be tested.
The first clamping unit is provided with a steam inlet, an exhaust port, a first cavity, a first annular groove, a first heat transfer medium inlet, a first heat transfer medium outlet and a temperature measuring port. The steam inlet is positioned at the top of the first clamping unit and is communicated with the first cavity. The steam inlet is connected with the one-way valve of the steam generating device through a pipeline and is used for introducing test gas into the test clamping device. The first annular groove is disposed around the first cavity and is not in communication with the first cavity. The first heat transfer medium inlet and the first heat transfer medium outlet are respectively communicated with the first annular groove. The first annular groove is configured to receive a heat transfer medium such that the test gas of the first cavity is maintained at a set temperature. The temperature measuring port is communicated with the first cavity and is used for measuring the temperature of the testing gas in the first cavity through the temperature measuring instrument. The exhaust port is in communication with the first cavity. The exhaust port is used for exhausting the residual testing gas in the first clamping unit.
The arrangement of the exhaust port can lead the application range of the test system to be wide, and can be used for accurately testing the protective performance of the breathable and semi-breathable materials.
The second clamping unit is provided with a vapor outlet, a displacement gas inlet, a second cavity, a second annular groove, a second heat transfer medium inlet and a second heat transfer medium outlet. The steam outlet is positioned at the bottom of the second clamping unit and is communicated with the second cavity. The vapor outlet is used for discharging the test gas permeated by the test sample. The second annular groove is disposed around the second cavity and is not in communication with the second cavity. The second annular groove is configured to receive a heat transfer medium such that the test gas within the second cavity is maintained at a set temperature. The second heat transfer medium inlet and the second heat transfer medium outlet are respectively communicated with the second annular groove. The replacement gas inlet is communicated with the second cavity and is used for completely replacing vapor in the second cavity, so that permeated test gas in the second cavity enters the sample injection switching device. The displacement gas may be an inert gas such as argon.
The second clamping unit and the first clamping unit are arranged substantially symmetrically. The first cavity and the second cavity have the same structure. In certain embodiments, the first cavity is isosceles triangle in cross-section.
The first annular groove and the second annular groove are provided with heat transfer medium, so that the test clamping device can maintain a constant test temperature, and the protective performance of the sample to be tested at a specific temperature can be measured. The heat transfer medium of the present invention may be water.
In the present invention, for heat preservation of the first cavity, the heat transfer medium enters from the first heat transfer medium inlet and flows out from the first heat transfer medium outlet. For the insulation of the second cavity, the heat transfer medium enters from the second heat transfer medium inlet and flows out from the second heat transfer medium outlet.
In certain embodiments, the first heat transfer medium outlet communicates with the second heat transfer medium inlet through a connection means. This is beneficial to maintaining consistency of temperature in the two cavities and saves resources.
The sealing unit is positioned below the sample to be tested. The sealing unit can enhance the degree of sealing between the first clamping unit and the second clamping unit. The sealing unit includes a first gasket and a second gasket. The first gasket and the second gasket are both disposed adjacent to the second clamping unit. The inner diameter of the first gasket is slightly larger than the maximum diameter of the cross section of the second cavity, and the outer diameter of the first gasket is smaller than the inner diameter of the second gasket. The outer diameter of the second gasket is smaller than the smallest diameter of the cross section of the second clamping unit. Thus, the tightness of the test clamping device is improved, and the test clamping device is convenient to install, clamp and detach the test sample to be tested.
The locking unit is connected with the first clamping unit and the second clamping unit respectively, and the locking unit can fix the first clamping unit and the second clamping unit. The locking unit comprises a first locking mechanism and a second locking mechanism. The first locking mechanism and the second locking mechanism are oppositely arranged. The first locking mechanism includes a bolt and an engagement member. The bolts are multiple, and the bolts can penetrate through the connecting piece and are fixed on the first clamping unit and the second clamping unit. The engagement member is foldable.
In some embodiments, the four bolts are provided, two of the four bolts respectively penetrate the engaging member and are fixed on the first clamping unit, and the other two bolts respectively penetrate the engaging member and are fixed on the second clamping unit, thereby fixing one side of the test clamping device.
In the invention, the connector is arranged to be foldable, which is advantageous in that the test clamping device forms a liftable cover structure. The arrangement of the connecting piece can enable the clamp to be hung on the testing instrument, for example, the clamp can be hung on the chemical vapor generator, and the operation is convenient.
The second locking mechanism includes a handle and a mating locking ring and shackle. The lock catch is arranged on the second clamping unit. The lock ring is connected with the handle. A portion of the handle is disposed on the first clamping unit. The second locking mechanism is used for locking the locking ring with the lock catch or separating the locking ring from the lock catch by operating the handle.
In the invention, when the handle is pulled outwards and downwards, the lock ring is separated from the lock catch, so that one side of the test clamping device is opened; when the handle is lifted, the lock ring is buckled with the lock catch, so that the test clamping device is locked and fixed. A rubber layer can be arranged on the handle to improve comfort. The handle can be properly prolonged, and the test clamping device can be easily opened by pulling the handle outwards. The lock catch can be a double-ring lock catch, and the stability of the locking unit is kept.
The joint unit is favorable for the communication of the test clamping device with the steam generating device and the sample injection switching device respectively through pipelines, and is favorable for the circulation of a heat transfer medium, the ventilation of replacement gas and the discharge of gas. The joint unit includes: the device comprises a vapor inlet connector connected with a vapor inlet, a vent connector connected with a vent, a first heat transfer medium inlet connector connected with a first heat transfer medium inlet, a first heat transfer medium outlet connector connected with a first heat transfer medium outlet, a temperature measuring port connector connected with a temperature measuring port, a vapor outlet connector connected with a vapor outlet, a replacement gas inlet connector connected with a replacement gas inlet, a second heat transfer medium inlet connector connected with a second heat transfer medium inlet and a second heat transfer medium outlet connector connected with a second heat transfer medium outlet.
In the invention, each connector is of a universal size, so that different related test instruments can be conveniently connected. The joint can be a two-way joint or a three-way joint and can be set according to actual needs. In some embodiments, the vapor inlet connector and the vapor outlet connector may be three-way connectors, wherein one end of the vapor inlet connector is connected with the vapor inlet, and the other end of the vapor inlet connector is used as a first pressure measuring port. One end of the steam outlet connector is connected with the steam outlet, and the other end of the steam outlet connector is used as a second pressure measuring port. The exhaust port connector can be a three-way connector, and one end of the exhaust port connector can be a pressure measuring port; the vent connector may also be a two-way connector.
Sample injection switching device
In some preferred embodiments, the system of the invention further comprises a sample injection switching device, so that a plurality of gas paths to be tested can be opened simultaneously, and the testing efficiency is improved.
The sample injection switching device is communicated with a plurality of steam outlets of a plurality of test clamping devices, and a plurality of gas paths to be tested are formed between the sample injection switching device and the steam outlets. The sample injection switching device is arranged to be capable of switching a plurality of gas paths to be tested, so that only one gas path to be tested is communicated with the online mass spectrum device at the same time. Therefore, a plurality of samples to be tested can be tested, the testing efficiency can be improved, and the use of equipment can be reduced.
In some embodiments, the sample switching apparatus has a plurality of test gas path inlets and a gas path outlet. The plurality of test gas path inlets are respectively communicated with the plurality of steam outlets. Thus, a plurality of gas paths to be tested can be formed between the steam outlet and the test gas path inlet. The gas path outlet is communicated with an online mass spectrum device, so that sample injection is convenient. A plurality of gas paths to be tested can be correspondingly formed between the plurality of test gas path inlets and one gas path outlet, and the sample injection switching device is arranged to enable only one gas path to be tested to be communicated with the online mass spectrum device at the same time.
The function of the sample injection switching device of the invention can be realized by adopting a multi-way switching control valve known in the art.
Online mass spectrum device
The invention adopts the online mass spectrum device to detect the permeated test gas, thereby improving the accuracy and the efficiency.
In some embodiments, the online mass spectrometry device is directly connected with the steam outlet of the test clamping device, and is suitable for detecting a single gas path to be tested.
In other embodiments, the online mass spectrometer device is connected with the sample injection switching device, and is used for quantitatively detecting permeated test gas, and is suitable for detecting a plurality of gas paths to be tested.
The ionization source of the online mass spectrum device can adopt electron bombardment ion source; the mass analyzer can adopt a three-stage filtering four-stage rod mass analyzer; the minimum data reading interval is less than or equal to 30s.
Compared with the traditional test paper or carbon tube adsorption weighing method, the method and the device can greatly improve the test accuracy and accurately judge the protection endpoint time by adopting the online mass spectrum device. Further preferably, the invention adopts the sample injection switching device and the online mass spectrum device, so that the test accuracy can be greatly improved, a plurality of samples to be tested can be measured at the same time, and the test efficiency is improved.
In the present invention, the breathable material and the semi-breathable material may be defined according to the standards in the art, and will not be described herein.
< test method >
The invention also provides a method for performing chemical vapor protection testing on a sample to be tested by adopting the system for testing the chemical vapor protection performance of the protective material. The following is a detailed description.
In certain embodiments, the method comprises the steps of:
step 1, setting corresponding parameters;
step 2, making the test gas containing chemical vapor generated by the vapor generating device reach the required concentration;
Step 3, mounting the sample to be tested in a test clamping device;
step 4, performing protection measurement on the sample to be tested;
and 5, after the measurement is finished, drawing a curve by taking time as an abscissa and taking a vapor concentration value as an ordinate, and obtaining a change curve of vapor permeation concentration along with time.
Wherein,
in step 1, the steam generator forms only one gas path pipeline for the test gas to circulate. The structures of the vapor generating device, the test clamping device and the online mass spectrometry device are as described above, and are not described in detail herein. In order to keep the test gas at a specific temperature, the connecting line may be coated with a heat trace. In step 1, the parameters include the concentration of chemical vapor of the test gas, the test temperature, and the relative humidity of the test gas. The setting of the parameters may be performed by a steam generating device.
In the step 2 and the step 3, after the concentration of the chemical vapor in the test gas containing the chemical vapor generated by the vapor generating device reaches the requirement, the test sample is installed. This ensures that the chemical vapor in the test gas begins to be tested at the set concentration.
In step 3, the sample to be tested is clamped between the first clamping unit and the second clamping unit, and the test clamping device is fixed.
In step 4, the test gas is introduced into the test clamping device from the vapor generating device, permeates through the sample to be tested, is discharged from the vapor outlet of the test clamping device, and is directly injected into the online mass spectrum device.
In other embodiments, the method of testing comprises the steps of:
s1, connecting a steam generating device, a test clamping device, a sample injection switching device and an online mass spectrum device in sequence through pipelines; starting the system, and setting corresponding parameters;
s2, enabling the test gas containing chemical vapor generated by the vapor generating device 1 to reach a set value;
s3, after the concentration of the chemical vapor reaches the set concentration, respectively installing a plurality of samples to be tested in a plurality of test clamping devices;
s4, performing protection measurement on the sample to be tested;
and S5, after the measurement is finished, drawing a curve by taking time as an abscissa and taking a vapor concentration value as an ordinate, and obtaining a change curve of vapor permeation concentration along with time.
In particular, the method comprises the steps of,
in S1, the steam generating device forms a plurality of parallel gas path pipelines for the test gas to circulate. The structures of the steam generating device, the test clamping device, the sample injection switching device and the online mass spectrum device are as described above, and are not described in detail herein. In order to keep the test gas at a specific temperature, the connecting line may be coated with a heat trace.
The parameters include the concentration of chemical vapor of the test gas, the test temperature, and the relative humidity of the test gas. The setting of the parameters may be performed by a steam generating device.
In S2 and S3, the test sample is mounted after the concentration of the chemical vapor in the test gas containing the chemical vapor generated by the vapor generating device is required. This ensures that the chemical vapor in the test gas begins to be tested at the set concentration.
And S3, clamping the sample to be tested between the first clamping unit and the second clamping unit and fixing the test clamping device.
S4, the test gas is respectively introduced into a plurality of test clamping devices from a plurality of gas path pipelines of the vapor generating device, is permeated through each test sample and is respectively discharged from vapor outlets of the plurality of test clamping devices to the sample injection switching device; the sample injection switching device automatically switches the gas paths to be tested at set interval time, so that only one gas path to be tested is communicated with the online mass spectrum device at the same time; the online mass spectrum device records the vapor signal value coming from the sample injection switching device in real time and converts the vapor signal value into a vapor concentration value.
In the invention, at least two gas paths to be tested can be more than three gas paths.
In certain embodiments, the switching interval between the gas paths to be tested is 30 seconds or more. The interval time can be determined according to the experimental time, and if the test time is long, the interval time can be correspondingly prolonged.
And S5, after the measurement is finished, drawing a curve by taking time as an abscissa and taking a vapor concentration value as an ordinate, and obtaining a change curve of the vapor permeation concentration along with the time.
In the present invention, the standard for ending the measurement is: after the vapor signal value no longer rises to stabilize, the test is stopped. In the invention, the protection end point time and integral C.t value of the sample to be tested can be obtained according to the curve. The greater these two values, the better the protective effect of the material.
The guard endpoint time is the time difference from the start of the test time to the point where the vapor concentration value no longer rises.
Example 1-System for testing chemical vapor barrier properties of barrier materials
Fig. 1 is a schematic structural diagram of a system for testing chemical vapor barrier properties of a barrier material according to the present invention. As shown in fig. 1, the system comprises a vapor generation device 1, a plurality of test clamping devices 2, a sample injection switching device 3 and an online mass spectrum device 4.
The vapor generating device 1 is used for generating a test gas. The vapor generating device 1 includes a chemical vapor generator 11, a humidity generator 12, a mixer 13, a flow meter 14, and a check valve 15.
The chemical vapor generator 11 is used for generating contaminated air containing chemical vapor. The humidity generator 12 is used to generate conditioned air. The mixer 13 is connected to the chemical vapor generator 11 and the humidity generator 12, respectively, for generating a test gas containing chemical vapor.
The mixer 13 is connected with a plurality of gas path pipelines which are arranged in parallel and used for the test gas to circulate. Preferably, the air path pipeline can be arranged to be 3. The flow meters 14 are arranged on the air path pipelines, and at least one flow meter 14 is arranged on each air path pipeline. The flow meter 14 is used to control the flow rate of the test gas. The check valve 15 is arranged on the air passage pipeline between the flowmeter 14 and the test clamping device 2, and each air passage pipeline is at least provided with one check valve 15. The check valve 15 controls the flow direction of the test gas. One end of the check valve 15 is connected with the flowmeter 14, and the other end of the check valve 15 is connected with the test clamping device 2. The vapor generating device 1 is also provided with a liquid crystal touch screen, and parameters such as temperature, relative humidity, flow rate and the like can be set through the liquid crystal touch screen.
The number of the test clamping devices 2 is consistent with the number of the air channel pipelines. Fig. 2 is a schematic structural diagram of a test clamping device according to the present invention. Fig. 4 is an exploded view of fig. 2. As shown in fig. 2 and 4, the test clamping device 2 includes a first clamping unit 21, a second clamping unit 22, a sealing unit 23, a locking unit 24, and a joint unit.
The first clamping unit 21 and the second clamping unit 22 are stacked, and the first clamping unit 21 is located above the second clamping unit 22, and the first clamping unit 21 and the second clamping unit 22 can clamp a sample to be tested.
Fig. 3 is a schematic cross-sectional view of a first clamping unit according to the present invention. As shown in fig. 3, the first clamping unit 21 is provided with a vapor inlet 211, an exhaust port (not shown), a first cavity 213, a first annular groove 214, a first heat transfer medium inlet (not shown), a first heat transfer medium outlet (not shown), and a temperature measuring port (not shown). The vapor inlet 211 is located at the top of the first clamping unit 21 and communicates with the first cavity 213. The steam inlet 211 is connected with a gas path pipeline of the steam generating device 1 and is used for introducing test gas into the test clamping device 2. The first annular groove 214 is disposed around the first cavity 213, and is not in communication with the first cavity 213. The first heat transfer medium inlet and the first heat transfer medium outlet are in communication with the first annular groove 214, respectively. The first annular groove 214 is capable of containing a heat transfer medium such that the test gas within the first cavity is maintained at a set temperature. The temperature measuring port is communicated with the first cavity 213 and is used for measuring the temperature of the testing gas in the first cavity 213 through a temperature measuring instrument. The exhaust port communicates with the first cavity 213. The exhaust port is used to exhaust the test gas remaining in the first clamping unit 21.
The second clamping unit 22 is provided with a vapor outlet (not shown), a displacement gas inlet (not shown), a second cavity (not shown), a second annular groove (not shown), a second heat transfer medium inlet (not shown), and a second heat transfer medium outlet (not shown). The steam outlet is positioned at the bottom of the second clamping unit and is communicated with the second cavity. The vapor outlet is used for discharging the test gas permeated by the test sample. The second annular groove is disposed around the second cavity and is not in communication with the second cavity. The second annular groove is configured to receive a heat transfer medium such that the test gas within the second cavity is maintained at a set temperature. The second heat transfer medium inlet and the second heat transfer medium outlet are respectively communicated with the second annular groove. The replacement gas inlet is communicated with the second cavity and is used for completely replacing the test gas in the second cavity, so that the test gas in the second cavity enters the sample injection switching device 3. The displacement gas may be an inert gas such as argon. The second clamping unit 21 and the first clamping unit 22 are arranged substantially symmetrically.
The sealing unit 23 is located below the sample to be measured. The sealing unit 23 can enhance the degree of sealing between the first clamping unit 21 and the second clamping unit 22. The sealing unit 23 includes a first gasket and a second gasket. Both the first gasket and the second gasket are disposed adjacent to the second clamping unit 22. The inner diameter of the first gasket is slightly larger than the maximum diameter of the cross section of the second cavity. The outer diameter of the first gasket is smaller than the inner diameter of the second gasket. The outer diameter of the second gasket is smaller than the smallest diameter of the cross section of the second clamping unit 22.
The locking unit 24 is connected to the first clamping unit 21 and the second clamping unit 22, respectively, and the locking unit 24 can fix the first clamping unit 21 and the second clamping unit 22. The locking unit 24 includes a first locking mechanism 241 and a second locking mechanism 242. The first locking mechanism 241 and the second locking mechanism 242 are disposed opposite to each other.
The first locking mechanism 241 includes a bolt and an engagement member 2411. The bolts are multiple. The bolts penetrate the engaging pieces 2411 and are fixed to the first clamping unit 21 and the second clamping unit 22. The engagement member 2411 can be folded.
The second locking mechanism 242 includes a handle 2421 and mating locking ring 2422 and lock 2423. The catch 2423 is provided on the second clamping unit 22. The lock ring 2422 is coupled to the handle 2421. A part of the handle 2421 is provided on the first clamping unit 21. The second locking mechanism 242 engages the catch 2422 with the catch 2423 or disengages the catch 2422 from the catch 2423 by manipulating the handle 2421.
The joint unit includes: a vapor inlet connection 101 connected to a vapor inlet 211, a vent connection 102 connected to a vent, a first heat transfer medium inlet connection 103 connected to a first heat transfer medium inlet, a first heat transfer medium outlet connection 104 connected to a first heat transfer medium outlet, a temperature sensing port connection 105 connected to a temperature sensing port, a vapor outlet connection 106 connected to a vapor outlet, a displacement gas inlet connection 107 connected to a displacement gas inlet, a second heat transfer medium inlet connection 108 connected to a second heat transfer medium inlet, and a second heat transfer medium outlet connection 109 connected to a second heat transfer medium outlet.
Fig. 5 is a schematic diagram of the working principle of a sample injection switching device of the present invention. As shown in fig. 5, the sample injection switching device 3 is communicated with the vapor outlet, and three gas paths to be tested, namely a path a, a path B and a path C, are respectively formed between the sample injection switching device and the vapor outlet. The sample injection switching device 3 can automatically switch the gas path to be tested after a program is set by software. The sample injection switching device 3 includes three test gas path inlets (the three test gas path inlets are an a path inlet a3, a B path inlet a1, and a C path inlet B4 respectively), a gas path outlet B3, a first exhaust hole a2, a second exhaust hole B1, a first connection hole a4, and a second connection hole B2. The first connection hole a4 and the second connection hole b2 communicate.
As shown in fig. 5 (1), during sampling on the a path (sampling on the B path and the C path is impossible, and only exhaust is possible), the permeated test gas enters the a path inlet a3 from the vapor outlet of one of the test clamping devices 2, then enters the first connecting hole a4, further enters the second connecting hole B2, and then exits from the gas path outlet B3, thereby sampling the on-line mass spectrometer 4. The B path is exhausted from the B path inlet a1 to the first exhaust hole a 2. The C path is exhausted from the C path inlet b4 to the second exhaust hole b 1.
As shown in fig. 5 (2), during sampling on the B path (the a path and the C path cannot sample, and only exhaust can be performed), the permeated test gas enters the B path inlet a1 from the vapor outlet of the other test clamping device 2, then enters the first connecting hole a4, further enters the second connecting hole B2, and then exits from the gas path outlet B3, so that the sample can be sampled to the online mass spectrometer 4. The a path is exhausted from the a path inlet a3 to the first exhaust hole a 2. The C path is exhausted from the C path inlet b4 to the second exhaust hole b 1.
As shown in fig. 5 (3), during sampling in the C path (the a path and the B path cannot sample, and only exhaust can be performed), the permeated test gas enters the C path inlet B4 from the vapor outlet of the further test clamping device 2, and then exits from the gas path outlet B3, so that the sample can be sampled into the online mass spectrometer 4. The a path is exhausted from the a path inlet a3 to the first exhaust hole a 2. The B path enters the first connecting hole a4 from the B path inlet a1, then enters the second connecting hole B2, and then is exhausted from the second exhaust hole B1.
The online mass spectrum device 4 is connected with the sample injection switching device 3 and is used for quantitatively detecting the permeated test gas. The ionization source of the online mass spectrum device of the embodiment can adopt electron bombardment ion source; the mass analyzer may employ a three-stage filtered four-stage rod mass analyzer.
Example 2
The protective material was subjected to chemical vapor barrier property test using the system for testing chemical vapor barrier property of protective material of example 1. The method comprises the following steps:
s1, starting all devices in the system, and setting corresponding parameters. In this embodiment, the number of air channels may be 3. The connecting pipeline is coated with a heat tracing belt, the temperature range is adjustable, and the test temperature of the embodiment is 30 ℃.
The sample to be tested in this example was a breathable material, and the chemical vapor for testing was set to dipropyl sulfide vapor. The chemical vapor concentration in the test gas was 2mg/L, the test temperature was 30℃and the relative humidity was 50%. The flow rate of the flowmeter is 600ml/min (three-way flow summation). S2, the test gas containing chemical vapor generated by the vapor generating device 1 is brought to a set value. In this example, the concentration of the chemical vapor was set to 2mg/L.
The chemical vapor generator 11 forms dipropyl sulfide into dipropyl sulfide vapor, and the contaminated air containing the dipropyl sulfide vapor is obtained. The humidity generator 12 generates conditioned air. The mixer 13 mixes the contaminated air containing dipropyl sulfide vapor from the chemical vapor generator 11 with the conditioned air from the humidity generator 12 to form a test gas.
In this embodiment, the online mass spectrometer 4 may be connected to the mixer 13, and the concentration of chemical vapor in the test gas may be quantitatively measured by the online mass spectrometer 4.
S3, after the concentration of the chemical vapor reaches the set concentration, three samples to be tested are respectively arranged in the three test clamping devices 2, so that the chemical vapor can be ensured to start the test of the samples to be tested under the specific concentration.
S4, performing protection measurement on the sample to be tested. The test gas is respectively introduced into the three test clamping devices 2 from the vapor generating device 1, permeates through the test sample to be tested and is discharged to the sample injection switching device 3 from a vapor outlet of the test clamping device 2; the sample injection switching device 3 automatically switches the gas paths to be tested at set interval time, so that only one gas path to be tested is communicated with the online mass spectrum device 4 at the same time. The online mass spectrometer 4 records the vapor signal value coming from the sample injection switching device 3 in real time and converts the vapor signal value into a vapor concentration value.
And S5, stopping the test after the steam signal value is not increased any more and is stable. And after the measurement is finished, drawing a curve by taking time as an abscissa and taking a vapor concentration value as an ordinate to obtain a change curve of the vapor permeation concentration along with the time.
The minimum data reading interval of the online mass spectrometry device 4 in this embodiment is 15s. FIG. 6 is a graph showing the change in vapor permeation concentration with time in example 2 of the present invention. FIG. 6 is a graph of test results for one of the test samples. As shown in fig. 6, the protection endpoint time and integral c·t value of the breathable material can be obtained from the curve. The unit of C is mg/m 3 The unit of time is min, the protection end point time is 70min, and the integral C.t value is 68480 mg.min/m 3 . The protection end-point time measured by the other two samples to be measured is 73min and 69min respectively; the integral C.t value is 69864 mg.min/m respectively 3 ，66854mg·min/m 3 。
Example 3
This embodiment differs from embodiment 2 only in that: the sample to be tested in this embodiment is a semi-permeable material, and the chemical vapor for testing is amyl sulfide vapor. The chemical vapor concentration in the test gas was 0.02mg/L and the relative humidity was 50%. The flow rate of the flowmeter is 600ml/min (three-way flow summation).
The chemical vapor generator 11 forms amyl sulfide vapor from amyl sulfide to obtain test gas containing amyl sulfide vapor. FIG. 7 is a graph showing the change in vapor permeation concentration with time in example 3 of the present invention. FIG. 7 is one of the standbyTest results graph of test specimen. As shown in FIG. 7, the semi-permeable material has a protection end point time of 1160min and an integral C.t value of 10480 mg.min/m 3 。
The protection end-point time measured by the other two samples to be measured is 1218min and 1079min respectively; the integral C.t. values were 10794 mg.min/m, respectively 3 ，10061mg·min/m 3 。
Example 4
The difference from embodiment 1 is that the steam generator 1 of this embodiment is formed with only one gas passage pipe through which the test gas flows. A flowmeter 14 and a one-way valve 15 are arranged on the air path pipeline in sequence. The test fixture 2 is one. The present embodiment does not include the sample switching apparatus 3. The steam generating device 1, the test clamping device 2 and the online mass spectrum device 4 are connected in sequence.
Example 5
The protective material was subjected to chemical vapor barrier property test using the system for testing chemical vapor barrier property of protective material of example 4. The types of the gas to be tested and the sample to be tested are the same as those of the embodiment 2, and the parameter setting is referred to the embodiment 2, and will not be described herein. The test method of the embodiment comprises the following steps:
step 1, starting each device in the system and setting corresponding parameters.
Step 2, the steam generator 1 is caused to generate a test gas containing chemical steam until the concentration of the chemical steam reaches the requirement.
And 3, installing a sample to be tested in the test clamping device 2.
And 4, performing protection measurement on the sample to be tested. That is, the test gas is introduced into the test clamping device 2 from the vapor generating device 1, permeates through the sample to be tested, is discharged from the vapor outlet of the test clamping device 2, and is introduced into the online mass spectrometer 4. The online mass spectrometry device 4 records the vapor signal value coming in from the vapor outlet in real time and converts the vapor signal value into a vapor concentration value.
And 5, stopping the test after the steam signal value is not increased any more and is stable. And after the measurement is finished, drawing a curve by taking time as an abscissa and taking a vapor concentration value as an ordinate to obtain a change curve of the vapor permeation concentration along with the time.
The protection endpoint time is 68min, and the integral C.t value is 66324 mg.min/m 3 . Compared with the embodiment 5, the embodiment 2 for simultaneously measuring three samples has no obvious difference, which shows that the combined use of the sample injection switching device 3 can improve the test efficiency under the condition of basically ensuring the accuracy.
Comparative example 1
The difference from example 2 is that protection tests were carried out using the method specified for the protection time of propane sulfide "gas-gas" in the GJB 3253-1998 flame retardant camouflage gas suit specification. The traditional protection test method is to use Congo red-chloramine indicator paper to change color to judge the endpoint, and only the endpoint can be judged qualitatively. The judged protection endpoint time is 63min.
The present invention is not limited to the above-described embodiments, and any modifications, improvements, substitutions, and the like, which may occur to those skilled in the art, fall within the scope of the present invention without departing from the spirit of the invention.
Claims (10)
1. A system for testing chemical vapor barrier properties of a barrier material, comprising:
a vapor generation device for generating a test gas containing chemical vapor;
a test clamping device comprising a first clamping unit and a second clamping unit; the first clamping unit and the second clamping unit are stacked, the first clamping unit is located above the second clamping unit, and the first clamping unit and the second clamping unit are arranged to be capable of clamping a sample to be tested; the first clamping unit is provided with a steam inlet and an exhaust port; the steam inlet is communicated with the steam generating device and is used for introducing test gas into the test clamping device; the second clamping unit is provided with a steam outlet; the vapor outlet is used for discharging the test gas penetrating through the sample to be tested; the exhaust port is used for exhausting the residual testing gas in the first clamping unit;
And the online mass spectrum device is connected with the vapor outlet and is used for quantitatively detecting the permeated test gas.
2. The system of claim 1, further comprising a sample switching device;
the steam generating device is provided with a plurality of parallel gas path pipelines for the test gas to circulate; the test clamping devices are arranged in a plurality, and each gas path pipeline is connected with a steam inlet of one test clamping device respectively;
the steam outlet of the test clamping device is connected with the online mass spectrum device through the sample injection switching device; the sample injection switching device is arranged to be capable of switching a plurality of gas paths to be tested, so that only one gas path to be tested is communicated with the online mass spectrum device at the same time.
3. The system according to claim 2, wherein:
the steam generating device further comprises a chemical steam generator, a humidity generator, a mixer, a plurality of flow meters and a plurality of one-way valves; wherein,
the chemical vapor generator is used for generating toxic air containing chemical vapor;
the humidity generator is used for generating air after humidity adjustment;
the mixer is respectively connected with the chemical vapor generator and the humidity generator and is used for generating test gas containing chemical vapor;
The gas path pipeline is connected with the mixer; each gas path pipeline is provided with a flowmeter and a one-way valve respectively; the flowmeter is used for controlling the flow rate of the test gas, and the one-way valve is used for controlling the flow direction of the test gas.
4. The system of claim 2, wherein the sample switching device has a plurality of test gas path inlets and a gas path outlet; the gas path outlet is connected with an online mass spectrum device; the plurality of test gas path inlets are respectively communicated with the plurality of steam outlets; a plurality of air paths to be tested can be correspondingly formed between a plurality of test air path inlets and one air path outlet.
5. The system of claim 1, wherein the test fixture further comprises a sealing unit and a locking unit,
the first clamping unit is further provided with a first cavity and a first annular groove; the steam inlet is positioned at the top of the first clamping unit and is communicated with the first cavity; the first annular groove is arranged around the first cavity and is not communicated with the first cavity; the exhaust port is communicated with the first cavity; the first annular groove is arranged to contain a heat transfer medium so that the test gas in the first cavity is maintained at a set temperature;
The second clamping unit is also provided with a second cavity and a second annular groove; the steam outlet is positioned at the bottom of the second clamping unit and is communicated with the second cavity; the second annular groove is arranged around the second cavity and is not communicated with the second cavity; the second annular groove is arranged to contain a heat transfer medium so that the test gas in the second cavity is maintained at a set temperature;
the sealing unit is positioned below the sample to be tested; the sealing unit is arranged to enhance the degree of sealing between the first clamping unit and the second clamping unit;
the locking unit is respectively connected with the first clamping unit and the second clamping unit, and the locking unit is arranged to be capable of fixing the first clamping unit and the second clamping unit.
6. The system according to claim 5, wherein:
the first clamping unit is also provided with a first heat transfer medium inlet, a first heat transfer medium outlet and a temperature measuring port; the first heat transfer medium inlet and the first heat transfer medium outlet are respectively communicated with the first annular groove; the temperature measuring port is communicated with the first cavity;
the second clamping unit is also provided with a second heat transfer medium inlet, a second heat transfer medium outlet and a replacement gas inlet; the second heat transfer medium inlet and the second heat transfer medium outlet are respectively communicated with the second annular groove; the displacement gas inlet is in communication with the second cavity.
7. The system of claim 5, wherein the locking unit comprises a first locking mechanism and a second locking mechanism; the first locking mechanism and the second locking mechanism are oppositely arranged; wherein,
the first locking mechanism comprises a bolt and an engagement piece; the bolts are arranged to penetrate through the connecting piece and are fixed on the first clamping unit and the second clamping unit; the connecting piece is arranged to be foldable;
the second locking mechanism comprises a handle and a lock ring and a lock catch which are matched with each other; the lock catch is arranged on the second clamping unit; the lock ring is connected with a handle, and a part of the handle is arranged on the first clamping unit; the second locking mechanism is configured to lock the shackle with the shackle or to separate the shackle from the shackle by operating the handle.
8. A method of chemical vapor protection testing a test sample using the system of claim 1, comprising the steps of:
step 1, setting corresponding parameters;
step 2, making the test gas containing chemical vapor generated by the vapor generating device reach the required concentration;
step 3, mounting the sample to be tested in a test clamping device;
Step 4, performing protection measurement on the sample to be tested;
and 5, after the measurement is finished, drawing a curve by taking time as an abscissa and taking the concentration value of the permeated test gas as an ordinate to obtain a change curve of the vapor permeation concentration along with the time.
9. A method of chemical vapor protection testing a test sample using the system of claim 2, comprising the steps of:
s1, setting corresponding parameters;
s2, enabling the test gas containing chemical vapor generated by the vapor generating device to reach the required concentration;
s3, respectively installing a plurality of samples to be tested in a plurality of test clamping devices;
s4, performing protection measurement on the sample to be tested;
and S5, after the measurement is finished, drawing a curve by taking time as an abscissa and taking a vapor concentration value as an ordinate, and obtaining a change curve of the vapor permeation concentration of the sample to be tested in the test clamping device along with the time.
10. The method according to claim 9, wherein:
in S1, the parameters include the concentration of chemical vapor in the test gas, the test temperature, and the relative humidity of the test gas;
s3, clamping the sample to be tested between the first clamping unit and the second clamping unit and fixing the test clamping device;
S4, the test gas is respectively introduced into a plurality of test clamping devices from a plurality of gas path pipelines of the vapor generating device, is permeated through each test sample and is respectively discharged from vapor outlets of the plurality of test clamping devices to the sample injection switching device; the sample injection switching device automatically switches the gas paths to be tested at set interval time, so that only one gas path to be tested is communicated with the online mass spectrum device at the same time; the online mass spectrum device records the vapor signal value coming in from the sample injection switching device in real time and converts the vapor signal value into a vapor concentration value;
in S5, after the vapor signal value no longer rises and becomes stable, the test is stopped.
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