CN203672755U - Gas transmission cell and determination device for determining film permeability characteristics of component gases of gas mixture simultaneously - Google Patents

Gas transmission cell and determination device for determining film permeability characteristics of component gases of gas mixture simultaneously Download PDF

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Publication number
CN203672755U
CN203672755U CN201320657769.1U CN201320657769U CN203672755U CN 203672755 U CN203672755 U CN 203672755U CN 201320657769 U CN201320657769 U CN 201320657769U CN 203672755 U CN203672755 U CN 203672755U
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gas
cell
sample
osmotic
test
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何建强
宋玉梅
刘利
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CHINA GUANGZHOU ANALYSIS & TEST CENTER
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CHINA GUANGZHOU ANALYSIS & TEST CENTER
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Abstract

The utility model discloses a gas transmission cell and a determination device for determining film permeability characteristics of component gases of a gas mixture simultaneously. According to the gas transmission cell and the determination device, a gas chromatograph and the gas transmission cell for determining the film permeability characteristics are combined, the permeability characteristics of multiple components of the gas mixture when the gas mixture penetrates through films and sheeting materials can be determined rapidly, accurately and simultaneously in one step, in addition, a gas blowing system is not required to be built, a quantitative sample feeding device is not required, the device can be used for determining the films with diameters of 8 mm and even smaller than 8 mm, and a gas chromatography flame ionization detector has adequate sensitivity when penetrating gases permeating for 5 min are tested. By means of the gas transmission cell and the determination device, mutual effects caused by the components on permeation rates when the gas mixture penetrates can be researched, and diffusion coefficients and solubility coefficients of the films and the sheeting materials can be determined conveniently.

Description

A kind of gas permeation pond and simultaneously measure the determinator that combination gas respectively forms the membrane permeability of gas
Technical field:
The utility model relates to and belongs to membrane material analysis and gas chromatographic analysis field, is specifically related to a kind of determinator that combination gas respectively forms the membrane permeability of gas of simultaneously measuring.
background technology:
At present, measure current the having much of proving installation of film and thin slice gas penetration potential.Test method ASTM D1434-82 (2009) e1 " standard method of plastic sheeting and thin slice ventilation characteristic measuring " (Standard Method for Determining Gas Permeability Characteristics of Plastic Film and Sheeting) of U.S.'s test and materialogy meeting, and the applied method of testing of the standard GB/T/T1038-2000 of China " plastic sheeting and thin slice gas-premeable test method pressure differential method " is pressure application.The gas penetration potential that these methods are measured film and thin slice is used the device or the similar device that are called gas permeation pond (Gas Transmission Cell), film or thin slice are sandwiched in wherein, allow gas to be measured pass into diaphragm one side, opposite side is measured the gas flow that sees through diaphragm by surveying instrument.But there is a common deficiency in these proving installations, can only measure a kind of gas penetration potential of gas, or the gas penetration potential that simultaneously sees through of mixed gas at every turn, can not once measure mixed gas simultaneously and see through time, mixed gas respectively forms the gas penetration potential of gas permeation film.In the time that reality is used many films be all in atmospheric environment or mixed-gas environment in, and mixed gas permeates owing to may there being influencing each other of gas, ventilative speed might not be in full accord while seeing through film with single composition of planting.
Another deficiency of at present conventional gas permeation system safety testing device is that test period is long, often needs a few hours to arrive tens of hours.
Visible, when mixed gas sees through, measure various gas permeance property is separately reality needs simultaneously, is also a difficult problem of measuring technology.
Gas chromatograph is a kind of reproducible, highly sensitive and modern analysis and test instrument that separating power is strong.
If gas permeation pond is received on gas chromatograph, utilize the carrier gas of gas chromatograph the gas that sees through film to be blown into the separation column cap of gas chromatograph, then select suitable method and chromatographic condition, can quick and precisely measure the gas penetration potential of film and thin slice, the perviousness of the various constituents of mixed gas of film or sheeting can also be once quick and precisely measure mixed gas and see through time simultaneously.
Patent CN102297827A discloses a kind of method of testing and test pool and proving installation of fuel cell film battery gas penetration potential, there is no thermostat, and the exit flow of inert gas is flowed directly into gas chromatograph injection port, need to bring the gas that sees through film into quantitative ring by sweep gas and test.But connection request is built a set of flow velocity and wanted little and steady sweep gas system like this, it is enough large that film permeation area is wanted, otherwise gas chromatograph detecting device does not have enough sensitivity accurately to test.This is not suitable for film, sheet material for testing small size.。
Patent CN202994616U discloses the gas permeation rate proving installation on a kind of gas permeation instrument, but has the problem that dead volume is large.
The common problem existing such as patent CN102297827A, CN202994616U and CN201314906Y has: the test gas cell cavity of (1) osmotic cell, and dead volume is unfavorable for greatly seeing through gas purging clean; (2) method of testing is that the gas that sees through during by stable seeing through is brought quantity tube into by the inert gas of continuous flow and purged into gas chromatograph for determination again, be enough to for reaching gas chromatograph the quantitative limit of measuring, it is enough large that the infiltrating area of film is wanted, and is not suitable for measuring film or the slow film of infiltration rate of small size; (3) need to set up the inert gas air supply system of flow speed stability; (4) be connected with gas phase easy not; (5) be difficult to calculate coefficient of diffusion.
Utility model content:
The purpose of this utility model is to provide a kind of determinator that combination gas respectively forms the membrane permeability of gas of simultaneously measuring, and has solved dead volume large, and the test duration is long, cannot accurate quantitative analysis; Easy not with gas chromatography connected mode, the problems such as inconvenient operation.
The utility model is achieved through the following technical solutions:
A kind of gas permeation pond, comprise osmotic cell base, there is the osmotic cell upper cover of symmetrical structure with osmotic cell base, the sealing gasket arranging between osmotic cell base and osmotic cell upper cover, osmotic cell base is connected by stationary installation with osmotic cell upper cover, described osmotic cell base is the reeded flat board of a side band with osmotic cell upper cover and groove is relative fastens, the surrounding of groove is amplexiformed mutually with membrane material to be measured, form disconnected two cell cavities mutually in the both sides of membrane material to be measured, be respectively the sample gas cell cavity of osmotic cell base and the test gas cell cavity of osmotic cell upper cover, the both sides, sample gas cell cavity bottom of described osmotic cell base are communicated with respectively the gas piping that runs through osmotic cell base, the both sides, test gas cell cavity bottom of described osmotic cell upper cover are communicated with respectively the gas piping that runs through osmotic cell upper cover, it is characterized in that described sample gas cell cavity and test gas cell cavity are all narrow strip (test gas cell cavity, long 1mm-300mm, wide 0.2mm-5mm, high 0.2mm-5mm, sample gas cell cavity, long 1mm-300mm, wide 0.2mm-5mm, high 1mm-30mm) and the gas piping of sample gas cell cavity and test gas cell cavity both sides be all located at the edge, bottom of groove, the gas seeing through is all blown into, reduce dead volume, go out peak sharp-pointed.
The sealing gasket arranging between described osmotic cell base and osmotic cell upper cover is preferably silicone rubber O-ring.
Described gas piping, can be the plastic tubes such as the metal tubes such as stainless steel, copper, aluminium or nylon, polypropylene, tygon, and in order to prevent from testing aspiration, to echo condensation can be pipeline set temperature control device as required.
Described mensuration combination gas respectively forms the determinator of the membrane permeability of gas, comprises that foregoing cell cavity is gas permeation pond, pressure control device, temperature control equipment, sample gas cylinder, four-way valve and the gas chromatograph of narrow strip; One end gas piping that the sample gas cell cavity bottom of described gas permeation pond base is provided with is sample gas air inlet pipeline, sample gas air inlet pipeline is communicated with sample gas cylinder through tensimeter, sample gas admittance valve, the other end gas piping of sample gas cell cavity bottom is sample gas outlet pipe, and sample gas outlet pipe is communicated with atmosphere through sample gas vent valve; The test air pipe that upper cover test both sides, gas cell cavity bottom, gas permeation pond are provided with connects respectively wherein two joints of four-way valve, one of them joint in two other joint of four-way valve is communicated with the gas-carrier pipeline of gas chromatograph, and another joint follows the chromatographic column of gas chromatograph to be communicated with by gas-carrier pipeline; Connection gas piping between sample gas cylinder, gas permeation pond is respectively equipped with valve, tensimeter forms pressure control device, is provided with in addition temperature control equipment.
Described four-way valve is external plane four-way sampling valve, or the six-way valve of the former outfit of gas chromatograph through shutoff the four-way valve that converts of sample gas inlet, outlet.
In order to increase the infiltrating area of membrane material, the gas permeation pond series connection of two above (comprising two) can be used if desired.
The beneficial effects of the utility model: the utility model utilizes gas chromatograph reproducible, highly sensitive, there is the feature of configuration the strong and many testing laboratories of separating power, the easy coupling that has realized gas chromatograph and surveyed the gas permeation pond of membrane permeability, the Multiple components perviousness of film and sheeting simultaneously while using this device can be once quick and precisely measure mixed gas to see through, and the utility model does not need to build the sweep gas system that needs accurate control flow, by turn four-way valve handle switching gas circuit, the carrier gas of gas chromatograph is switched to the osmotic cell test gas cell cavity of flowing through and enters again chromatographic column, utilize the carrier gas of gas chromatography by quick from test gas cell cavity the test gas that sees through film, all be blown into chromatographic column and carry out gas chromatographic analysis, do not need through quantitative sampling device, can be used for the film that test diameter 8mm is even less, the test infiltration gas that sees through of 5 minutes has had enough sensitivity with gas chromatographic flame ionization detector.Utilize the utility model, can study mixed gas and see through time, various compositions, to the influencing each other of infiltration rate, can conveniently record coefficient of diffusion and the solubility coefficient of film and sheeting.
Brief description of the drawings:
Fig. 1 is the utility model vapor-phase chromatography special gas osmotic cell schematic diagram;
Fig. 2 is that the utility model is measured the connection diagram that combination gas respectively forms the device of the membrane permeability of gas;
Fig. 3 is the utility model process of osmosis and sample introduction analytic process schematic diagram;
Wherein: 1. sample gas vent valve, 2. sample gas outlet pipe, 3. osmotic cell, 4. test air pipe, 5. four-way valve, 6. gas-carrier pipeline, 7. sample gas gas admittance valve, 8. tensimeter, 9. sample gas air inlet pipeline, 10. osmotic cell attemperating unit, 11. test air pipes, 12. gas-carrier pipeline, 13. gas chromatographs, 14. test gas cell cavities, 15. sample gas cell cavities, 16. films to be measured, 17. sealing gaskets, 18. osmotic cell upper covers, 19. osmotic cell bases, 20. chromatographic columns.
embodiment:
Below to further illustrate of the present utility model, instead of to restriction of the present utility model.
Embodiment 1:
When seeing through polyethylene film, liquefied petroleum gas (LPG) measures the wherein infiltrative gas Chromatographic Determination device of propane, normal butane and isobutane simultaneously
The present embodiment adopts the vapor-phase chromatography special gas osmotic cell of a fillet type cell cavity, sees Fig. 1.This gas permeation pond 3 comprise osmotic cell base 19, and osmotic cell base 19 there is the sealing gasket 17 arranging between osmotic cell upper cover 18, osmotic cell base 19 and the osmotic cell upper cover 18 of symmetrical structure, osmotic cell base 19 and osmotic cell upper cover 18 are equipped with screw, fix by screw bolt and nut; Described osmotic cell base 19 and osmotic cell upper cover 18 are the reeded flat board of a side band, and groove fastens relatively, the surrounding of groove is amplexiformed mutually with membrane material to be measured, form disconnected two cell cavities mutually in the both sides of membrane material to be measured, be respectively the sample gas cell cavity 15 of osmotic cell base 19 and the test gas cell cavity 14 of osmotic cell upper cover 18, sample gas cell cavity 15 both sides, bottom of described osmotic cell base 19 are communicated with respectively the gas piping 2 and 9 that runs through osmotic cell base 19; Test gas cell cavity 14 both sides, bottom of described osmotic cell upper cover 18 are communicated with respectively the gas piping 4 and 11 that runs through osmotic cell upper cover; Described sample gas cell cavity and test gas cell cavity are all narrow strip, length × wide × height=8.12mm × 0.90mm × 2.00mm, and the gas piping of sample gas cell cavity 15 and test gas cell cavity 14 both sides is all located at the edge, bottom of groove, and the gas seeing through is all blown into, reduce dead volume, go out peak sharp-pointed.
When use, in gas permeation pond, base 19 inside surfaces are coated vacuum grease, load onto the silicone rubber seal gasket 17 that has through hole at infiltration chamber correspondence position, sealing gasket 17 upper sides are put film 16 to be measured after coating vacuum grease, be loaded on the osmotic cell upper cover 18 that inside surface scribbles vacuum grease, with fastened by screw, the gas permeation pond that obtains assembling; Be placed in thermostatic bath 10 and carry out constant temperature test.In the time that the PE film with thickness 0.04mm is made liquefied petroleum permeability to gas mensuration, the minimum time of penetration that gas chromatography hydrogen flame detector can obviously be measured seen through liquefied petroleum gas (LPG) composition is not more than 15 minutes.
The device that described mensuration combination gas respectively forms the membrane permeability of gas connects by Fig. 2.Comprise that cell cavity is gas permeation pond 3, pressure control device, temperature control equipment, sample gas cylinder, four-way valve 5 and the gas chromatograph 13 of narrow strip.
One end gas piping that sample gas cell cavity 15 bottoms of described gas permeation pond base 19 are provided with is sample gas air inlet pipeline 9, sample gas air inlet pipeline 9 is communicated with sample gas cylinder through tensimeter 8, sample gas gas admittance valve 7, the other end gas piping of sample gas cell cavity bottom is sample gas outlet pipe 2, and sample gas outlet pipe 2 is communicated with atmosphere through sample gas vent valve 1; Gas permeation pond upper cover 18 is tested wherein two joints that test air pipe 4 and 11 that gas cell cavity 14 both sides, bottom are provided with is connected respectively four-way valve 5, one of them joint in two other joint of four-way valve 5 is communicated with the gas-carrier pipeline 6 of gas chromatograph 13, another joint is communicated with and obtains measuring the device that combination gas respectively forms the membrane permeability of gas with the chromatographic column of gas chromatograph 13 by gas-carrier pipeline 12, is placed in thermostatic bath constant temperature.
Connection gas piping between sample gas cylinder, gas permeation pond is respectively equipped with valve, tensimeter forms pressure control device, is provided with in addition temperature control equipment.
Described gas permeation pond can be two or more.
When test, first opening sample gas gas admittance valve 7 passes into sample gas and drives other gases in gas permeation pond sample gas cell cavity 15 and gas piping 2 and 9 away, turn four-way valve 5 handles enter chromatographic column after the carrier gas of gas chromatograph 13 is switched to gas coming through osmotic cell test gas cell cavity 14 again, logical carrier gas 30s drives away after the gas in test gas cell cavity 14, turn four-way valve 5 handles switch back the carrier gas of gas chromatograph 13 directly to enter chromatographic column again, start to calculate time of penetration simultaneously.After sample gas infiltration certain hour infiltration rate is stable, turn four-way valve 5 handles are switched to by the carrier gas of gas chromatograph 13 the osmotic cell test gas cell cavity 14 of flowing through and enter chromatographic column again, sweep gas chromatograph and carry out gas chromatographic analysis (Fig. 3 is shown in by process of osmosis and sample introduction analytic process schematic diagram) with carrier gas by penetrating film to the test air-blowing in test gas cell cavity; Record thickness, film infiltrating area, sample gas pressure, room temperature, thermostatic bath temperature, gas chromatography test condition, calculate film infiltration coefficient according to chromatogram.
Described optimum GC conditions is:
Chromatographic column: SE-30 capillary column (50mm × 0.32mm × 1um);
Carrier gas: nitrogen;
Detecting device: flame ionization detector;
Detector temperature: 200 DEG C;
Injector temperature: 150 DEG C;
Column temperature: 35 DEG C;
Post flow: 1.0ml/min;
Input mode: split sampling, split ratio 30:1;
Tail blows: 25ml/min.
Embodiment 2: simultaneously measure film, the infiltrative proving installation of sheet material multicomponent while utilizing the repacking of gas chromatograph first wife six-way valve to see through for mixed gas
Now gas chromatograph polygamy has six-way valve, measures film, sheet material multicomponent perviousness while can simple refit becoming four-way valve to see through for mixed gas simultaneously.Back out first wife's six-way valve for connecing two collar nuts of sample tracheae, with silicon rubber plug, these two joints of six-way valve are blocked respectively.Pull down the quantitative ring of six-way valve, replace quantitatively and encircling with osmotic cell in Fig. 1, osmotic cell is tested to air pipe 4 and 11 and be connected to the former joint that connects quantitative ring of six-way valve.All the other analytical approachs and operation steps are with embodiment 1.

Claims (7)

1. a gas permeation pond, comprise osmotic cell base, there is the osmotic cell upper cover of symmetrical structure with osmotic cell base, the sealing gasket arranging between osmotic cell base and osmotic cell upper cover, osmotic cell base is connected by stationary installation with osmotic cell upper cover, described osmotic cell base is the reeded flat board of a side band with osmotic cell upper cover and groove is relative fastens, the surrounding of groove is amplexiformed mutually with membrane material to be measured, form disconnected two cell cavities mutually in the both sides of membrane material to be measured, be respectively the sample gas cell cavity of osmotic cell base and the test gas cell cavity of osmotic cell upper cover, both sides, described sample gas cell cavity bottom are communicated with respectively the gas piping that runs through osmotic cell base, both sides, described test gas cell cavity bottom are communicated with respectively the gas piping that runs through osmotic cell upper cover, it is characterized in that gas piping that described sample gas cell cavity and test gas cell cavity are all narrow strip and sample gas cell cavity and test gas cell cavity both sides is all located at the edge, bottom of groove.
2. gas permeation according to claim 1 pond, is characterized in that, described sealing gasket is silicone rubber O-ring.
3. gas permeation according to claim 1 pond, is characterized in that, described gas piping is metal tube or plastic tube and is provided with temperature control equipment.
4. gas permeation according to claim 1 pond, is characterized in that, described test gas cell cavity, long 1mm-300mm, wide 0.2mm-5mm, high 0.2mm-5mm, described sample gas cell cavity, long 1mm-300mm, wide 0.2mm-5mm, high 1mm-30mm.
5. measure the determinator that combination gas respectively forms the membrane permeability of gas for one kind simultaneously, it is characterized in that, comprise the gas permeation pond described in any one claim, pressure control device, temperature control equipment, sample gas cylinder, four-way valve and gas chromatograph in claim 1-4; The sample gas air inlet pipeline that the sample gas cell cavity bottom of described gas permeation pond base is provided with is communicated with sample gas cylinder through tensimeter, sample gas admittance valve, and the sample gas outlet pipe of sample gas cell cavity bottom is communicated with atmosphere through sample gas vent valve; The test air pipe that upper cover test both sides, gas cell cavity bottom, gas permeation pond are provided with connects respectively wherein two joints of four-way valve, one of them joint in two other joint of four-way valve is communicated with the gas-carrier pipeline of gas chromatograph, and another joint follows the chromatographic column of gas chromatograph to be communicated with by gas-carrier pipeline; Connection gas piping between sample gas cylinder, gas permeation pond is respectively equipped with valve, tensimeter forms pressure control device, is provided with in addition temperature control equipment.
6. according to claim 5ly measure the determinator that combination gas respectively forms the membrane permeability of gas simultaneously, it is characterized in that, described four-way valve is external plane four-way sampling valve, or the six-way valve of the former outfit of gas chromatograph through shutoff the four-way valve that converts of sample gas inlet, outlet, again or the good four-way valve of other gas tightness.
7. according to claim 5ly measure the determinator that combination gas respectively forms the membrane permeability of gas simultaneously, it is characterized in that, described gas permeation pond is one or more.
CN201320657769.1U 2013-10-23 2013-10-23 Gas transmission cell and determination device for determining film permeability characteristics of component gases of gas mixture simultaneously Expired - Lifetime CN203672755U (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103575630A (en) * 2013-10-23 2014-02-12 中国广州分析测试中心 Measuring method and device for simultaneously measuring membrane permeability of each gas mixed gas
CN107328703A (en) * 2017-08-21 2017-11-07 中国计量科学研究院 A kind of preparation method of reusable gas permeation rate reference membrane
CN110618077A (en) * 2019-09-19 2019-12-27 东华大学 Device and method for measuring dynamic air filtering and isolating efficiency of fabric and application
CN110618076A (en) * 2019-09-19 2019-12-27 东华大学 Double-cylinder axial moving bulging type fabric air-lock and air-filtration performance measuring device and method

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103575630A (en) * 2013-10-23 2014-02-12 中国广州分析测试中心 Measuring method and device for simultaneously measuring membrane permeability of each gas mixed gas
CN103575630B (en) * 2013-10-23 2016-04-27 中国广州分析测试中心 A kind of Simultaneously test combination gas respectively forms the assay method of the membrane permeability of gas
CN107328703A (en) * 2017-08-21 2017-11-07 中国计量科学研究院 A kind of preparation method of reusable gas permeation rate reference membrane
CN110618077A (en) * 2019-09-19 2019-12-27 东华大学 Device and method for measuring dynamic air filtering and isolating efficiency of fabric and application
CN110618076A (en) * 2019-09-19 2019-12-27 东华大学 Double-cylinder axial moving bulging type fabric air-lock and air-filtration performance measuring device and method
CN110618077B (en) * 2019-09-19 2021-12-10 东华大学 Device and method for measuring dynamic air filtering and isolating efficiency of fabric and application
CN110618076B (en) * 2019-09-19 2022-07-15 东华大学 Double-cylinder axial moving bulging type fabric air-lock and air-filtration performance measuring device and method

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