CN109632600B - Trace oxygen transmission rate testing method - Google Patents
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 174
- 239000001301 oxygen Substances 0.000 title claims abstract description 174
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 174
- 238000012360 testing method Methods 0.000 title claims abstract description 45
- 230000005540 biological transmission Effects 0.000 title claims abstract description 24
- 238000001514 detection method Methods 0.000 claims abstract description 15
- 239000007789 gas Substances 0.000 claims abstract description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 78
- 229910052757 nitrogen Inorganic materials 0.000 claims description 34
- 238000000034 method Methods 0.000 claims description 16
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 10
- 238000010998 test method Methods 0.000 claims description 5
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 2
- 229910001882 dioxygen Inorganic materials 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 15
- 238000004458 analytical method Methods 0.000 abstract description 5
- 230000002035 prolonged effect Effects 0.000 abstract description 3
- 230000004888 barrier function Effects 0.000 description 10
- 230000008569 process Effects 0.000 description 10
- 238000010586 diagram Methods 0.000 description 5
- 239000012466 permeate Substances 0.000 description 5
- 239000005022 packaging material Substances 0.000 description 4
- 230000000149 penetrating effect Effects 0.000 description 4
- 238000005070 sampling Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 230000009471 action Effects 0.000 description 2
- 230000001174 ascending effect Effects 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003204 osmotic effect Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- 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
- G01N15/0806—Details, e.g. sample holders, mounting samples for testing
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- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
- Investigating Or Analyzing Materials By The Use Of Electric Means (AREA)
- Investigating Or Analyzing Materials By The Use Of Fluid Adsorption Or Reactions (AREA)
Abstract
The invention discloses an oxygen transmission rate testing method, which can effectively avoid the phenomena of incapability of detecting test data, large fluctuation, poor reproducibility and the like caused by the fact that the concentration of oxygen can not reach the detection lower limit of an oxygen sensor when a high-barrier material is tested by enriching gas and sending oxygen permeating a sample to the oxygen sensor for analysis when the detection limit of the sensor or a higher range is reached, and improve the detection accuracy. In order to protect the oxygen sensor, a valve III is added in front of the oxygen sensor, a bypass step is added, the impact of high-concentration oxygen sealed in air on the oxygen sensor when a sample is clamped is prevented, and the service life of the oxygen sensor is prolonged.
Description
Technical Field
The invention relates to a trace oxygen transmittance testing method, and belongs to the technical field of material transmittance testing methods.
Background
The barrier property of the material to oxygen is an important index for measuring whether the material is suitable for certain fields: for packaging materials, the shelf life of the goods in the package is directly influenced; the basic method of testing a material for oxygen permeability (i.e., the barrier of the material to oxygen) is to test the oxygen content of the gas that permeates through the material. The testing method has a plurality of types, and the oxygen resistance of the packaging material detected by the electrochemical oxygen sensor is determined by national and international relevant standards.
In the traditional test method, a permeation chamber is divided into a permeation upper chamber and a permeation lower chamber, a sample is clamped between the upper chamber and the lower chamber during test, and the permeation chamber is divided into two independent sealed chambers by the sample. The upper permeation cavity is provided with two air holes, one air hole is connected with an oxygen source, the other air hole is an exhaust hole, and the oxygen exhaust hole is connected with the atmosphere. The permeation lower cavity is also provided with two air holes, one air hole is connected with a high-purity nitrogen gas source, and the other air hole is a nitrogen gas outlet connected with an oxygen sensor. During the test, oxygen with continuous rated flow rate flows through the upper permeation cavity, high-purity nitrogen with continuous rated flow rate flows through the lower permeation cavity, oxygen molecules penetrate through the sample to reach the lower permeation cavity due to the fact that oxygen concentration difference exists on two sides of the sample, the oxygen molecules penetrating into the lower permeation cavity are carried to the oxygen sensor by the flowing high-purity nitrogen, the size of signals generated by the oxygen sensor is in direct proportion to the amount of the oxygen penetrating into the lower permeation cavity, and indexes such as the oxygen transmission rate of the sample can be obtained through calculation of the oxygen signal variation in unit time.
However, for medium-low barrier materials and a part of high barrier materials, the traditional oxygen transmission rate testing device can still meet the testing requirements, but for a considerable part of high barrier materials or ultrahigh barrier materials, the traditional oxygen transmission rate testing device is useless, and accurate data is difficult to obtain, because the detection limit of the oxygen sensor cannot be low enough, the amount of oxygen permeating through a high barrier sample is extremely trace, the oxygen sensor cannot identify the extremely trace oxygen, even the generated signals are submerged by noise, and macroscopically, the phenomena that the testing data cannot be detected, the fluctuation is large, the reproducibility is poor and the like are shown; in order to improve the detection limit of the oxygen sensor, the development speed of the barrier property of the material is obviously higher than that of the oxygen sensing technology at present, based on innovation and breakthrough in the sensing field.
The food and medicine spoilage is expected in the future, the oxygen or water vapor entering in the packaging link is the most important reason for the failure of the quality guarantee period, the stronger the oxygen and water vapor blocking capacity of the packaging material is, the longer the product quality guarantee period can be obtained by the packaged contents, and the higher the demand of social development on the barrier property of the packaging material is; in the field of new materials and new energy, the barrier property of some materials can reach 10-4- 10-5ml/m2.d, whereas the detection limit of conventional oxygen transmission rate testing techniques is typically 10-2- 10-3ml/m2.d, and 2-3 magnitude order difference from the testing requirement, therefore, the traditional oxygen transmission rate testing method is difficult to meet the packaging requirement of the current era, and based on the development breakthrough of the sensor, the method is a long waiting process, and the requirement is current, and the technical innovation is imperative.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a trace oxygen transmission rate testing method, trace water vapor penetrating through a sample is enriched, and when the trace water vapor is enriched to the detection limit or a higher range of a sensor, oxygen penetrating through the sample is sent to the oxygen sensor for analysis, so that the accuracy of the oxygen transmission rate testing result is improved.
In order to solve the problems, the invention adopts the technical scheme that: a trace oxygen transmission rate testing method comprises the following steps: s01), the air inlet pipeline and the air outlet pipeline of the permeation lower cavity are communicated with the permeation lower cavity, the pipeline between the air outlet pipeline and the oxygen sensor is disconnected and emptied, the oxygen source is opened, oxygen flows in the permeation upper cavity, the nitrogen source is opened, and nitrogen entering the permeation lower cavity through the air inlet pipeline carries air in the permeation lower cavity to be discharged from the air outlet pipeline;
s02), communicating an air inlet pipeline and an exhaust pipeline of the permeation lower cavity with the permeation lower cavity, communicating the exhaust pipeline with a pipeline between oxygen sensors, transmitting nitrogen entering the permeation lower cavity from a nitrogen source to the oxygen sensors through the exhaust pipeline, keeping the state, and recording the value Tx-Z0 of the oxygen sensors until the oxygen sensing signal peak is finished;
s03), the air inlet pipeline and the exhaust pipeline of the permeation lower cavity are disconnected with the permeation lower cavity, the permeation lower cavity forms a completely sealed cavity V1, the pipelines from the exhaust pipeline to the oxygen sensor are communicated, and nitrogen entering the air inlet pipeline directly enters the oxygen sensor to perform zero point test;
s04), keeping the state of the step S03, so that oxygen molecules permeating the sample can be enriched in the sealed chamber V1 to ensure that the oxygen amount permeating can completely enter the effective detection range of the oxygen sensor, and recording the zero point value of the oxygen sensor at the moment as Z0;
s05), repeat steps S02 through S04 until S =
The value is stable, and S is the value of oxygen transmission rate.
The on-off of the pipelines from the permeation lower cavity air inlet pipeline, the exhaust pipeline and the exhaust pipeline to the oxygen sensor is controlled by valves arranged on the permeation lower cavity air inlet pipeline and the exhaust pipeline.
The gas inlet pipeline of the permeation lower cavity is provided with a valve I, the gas outlet pipeline of the permeation lower cavity is provided with a valve II and a valve III, the valve I, the valve II and the valve III are all three-way valves, the end a of the valve I is communicated with a nitrogen gas source, the end c is communicated with the inlet of the permeation lower cavity, the end c of the valve II is communicated with the outlet of the permeation lower cavity, the end a is communicated with the end a of the valve III, the end c of the valve III is communicated with an oxygen sensor, the ends I and b of the valve I are communicated with the end b of the valve II, the end b of the valve III is suspended, and only one way of the three-way.
The gas inlet pipeline of the permeation lower cavity is provided with a valve I, the gas exhaust pipeline of the permeation lower cavity is provided with a valve II and a valve III, the gas inlet pipeline and the gas exhaust pipeline are provided with a valve IV, the valve I, the valve II and the valve IV are all two-way valves, the valve III is a three-way valve, the front end of the valve I is communicated with a nitrogen gas source, the rear end of the valve I is communicated with an inlet of the permeation lower cavity, the front end of the valve II is communicated with an outlet of the permeation lower cavity, the rear end of the valve II is communicated with an a end of the valve III, a c end of the valve III is communicated with an oxygen sensor, a b end of the valve III is suspended, and.
The invention has the beneficial effects that: according to the invention, by enriching the gas, when the detection limit of the sensor or a higher range is reached, the oxygen permeating the sample is sent to the oxygen sensor for analysis, so that the phenomena of incapability of detecting test data, large fluctuation, poor repeatability and the like caused by the fact that the concentration of the oxygen cannot reach the detection limit of the oxygen sensor during the test of the high-barrier material can be effectively avoided, and the detection accuracy is improved. In order to protect the oxygen sensor, a valve III is added in front of the oxygen sensor, a bypass step is added, the impact of high-concentration oxygen sealed in air on the oxygen sensor when a sample is clamped is prevented, and the service life of the oxygen sensor is prolonged.
Drawings
FIG. 1 is a schematic structural diagram of a testing apparatus used in the testing method described in embodiment 1;
FIG. 2 is a schematic structural diagram of a testing apparatus used in the testing method described in embodiment 2;
FIG. 3 is a schematic diagram of the oxygen sensor detecting the change of oxygen concentration during the sampling analysis stage;
FIG. 4 is a schematic diagram of the oxygen sensor detecting changes in oxygen concentration during the enrichment process;
in the figure: 1. the device comprises a permeation upper chamber, 2 permeation lower chamber, 3 permeation upper chamber air inlet pipe, 4 permeation upper chamber exhaust pipe, 5 permeation lower chamber air inlet pipe, 6 permeation lower chamber exhaust pipe, 7 oxygen gas source, 8 nitrogen gas source, 9 valve I, 10 valve II, 11 valve III, 12 valve IV, 13 valve oxygen sensor, 14 and a sample.
Detailed Description
The invention is further described with reference to the following figures and specific embodiments.
Example 1
The embodiment discloses a trace oxygen transmission rate testing method, which is based on a testing device shown in fig. 1, a valve I9 is arranged on an air inlet pipeline 5 of a permeation lower cavity 2, a valve II10 and a valve III11 are arranged on an exhaust pipeline 6 of the permeation lower cavity 2, the valve I9, the valve II10 and the valve III11 are all three-way valves, an end a of the valve I9 is communicated with a nitrogen gas source 8, an end c of the valve I9 is communicated with an inlet of the permeation lower cavity 2, an end c of the valve II10 is communicated with an outlet of the permeation lower cavity 2, an end a of the valve III11 is communicated with an end a of the valve III11, an end c of the valve I9 and an end b of the valve II10 are communicated, an end b of the valve III11 is suspended, only one way of the three-way valve is communicated in one state, or ab is communicated, and ac is communicated with ab, and ac is communicated with ac.
The test method of the embodiment specifically comprises the following steps:
s01) and a bypass, wherein the end a and the end c of the valve I, II are communicated, the end a and the end b of the valve III11 are communicated, the air inlet pipeline 5 and the exhaust pipeline 6 of the permeation lower cavity 2 are communicated at the moment, the pipeline between the exhaust pipeline 6 and the oxygen sensor 13 is disconnected, the oxygen source 7 is opened, oxygen flows in the permeation upper cavity 1, the nitrogen source 8 is opened, and nitrogen entering the permeation lower cavity 2 through the air inlet pipeline 5 carries air in the permeation lower cavity 2 to be exhausted from the exhaust pipeline 6;
s02), sampling and analyzing, keeping the conduction of the air inlet pipeline 5 and the exhaust pipeline 6 of the permeation lower cavity 2, switching a valve III11 to enable ac to be communicated, conducting the pipeline between the exhaust pipeline 6 and the oxygen sensor 13, enabling oxygen permeating the upper cavity 1 to permeate the sample 14 to reach the permeation lower cavity 2, transmitting the permeated oxygen to the oxygen sensor 13 by the nitrogen entering the permeation lower cavity 2 from the nitrogen source 8, and when the oxygen sensor 13 detects that the value of the oxygen content in the nitrogen exceeds a zero point Z0Recording the time at this time as t1After a period of time, when the oxygen content in the nitrogen gas is reduced to zero point Z0At the moment, record thisTime of day is t2Simultaneously recording t1To t2Value T of staged oxygen sensorxAnd calculate Tx-Z0The oxygen concentration changes during this process as shown in fig. 3.
S03), starting enrichment and zero point test, switching a valve I9 to enable ab to be communicated, switching a valve II10 to enable ba to be communicated, keeping a valve III11 communicated with ac, disconnecting an air inlet pipeline 5 and an exhaust pipeline 6 of a permeation lower cavity 2, and conducting a pipeline between the exhaust pipeline 6 and an oxygen sensor 13, wherein the valve I9, the permeation lower cavity 2 and a valve II10 form a completely sealed cavity V1, and the sealed cavity is filled with high-purity nitrogen; the flowing high-purity nitrogen reaches the oxygen sensor through ab of the valve I9, ba of the valve II10 and ac of the valve III11, and the oxygen sensor test is oxygen in the high-purity nitrogen, namely, the zero point test;
s04) and S03, under the action of the oxygen concentration difference on two sides of the sample, oxygen permeates from the high-concentration side to the low-concentration side of the sample 14, oxygen molecules permeating through the sample 14 are enriched in the sealed chamber V1, the oxygen content of the sealed chamber V1 is higher and higher along with the prolonging of time, and the enrichment time is determined according to the permeation rate of the sample, so that the oxygen content permeating can completely enter the effective detection range of the oxygen sensor. After the set time is reached, the process proceeds to step S02.
S05), repeating steps S02 to S04 according to S =
And calculating the value of the oxygen transmission rate until the value of S is stable, wherein S is the value of the oxygen transmission rate.
Since there may be a trace of oxygen in the high purity nitrogen, Z is zero point tested0The value is not zero but is a constant and stable constant, and the oxygen concentration changes during the enrichment process as shown in fig. 4. For accurate calculation of the value of oxygen transmission rate, Z is subtracted from the detected sensor signal value Tx0The value is obtained, and the real area of the electric signal area of the sensor can be obtained.
During the enrichment process, the lower osmotic cavity 2 is enriched with more oxygen, so thatWhen the enrichment waiting step is shifted to the sampling analysis stage, the oxygen concentration detected by the oxygen sensor is in an ascending process, in the process, the valve I9 and the valve II10 are both in an opening state, the enrichment effect is lost, the oxygen permeation permeating the upper chamber 1 is slow, after the ascending stage, the oxygen concentration detected by the oxygen sensor 13 is reduced, the specific schematic diagram is shown in fig. 3, and t is calculated1To t2The total amount of oxygen transmitted between is the oxygen transmission rate of the sample.
When the sample is clamped, the lower permeation cavity 2 is filled with air, the oxygen concentration in the air is high-concentration oxygen relative to the oxygen permeated by the sample, and in order to protect the oxygen sensor 13, the high-concentration oxygen in the lower permeation cavity of the lower permeation cavity needs to be purged out through a bypass step, so that the service life of the oxygen sensor is prolonged.
Example 2
The embodiment discloses a trace oxygen permeability testing method, which is based on a testing device shown in fig. 2, a valve I9 is arranged on an air inlet pipeline 5 of a permeation lower cavity 2, a valve II10 and a valve III11 are arranged on an air exhaust pipeline 6 of the permeation lower cavity 2, a valve IV12 is arranged between the air inlet pipeline 5 and the air exhaust pipeline 6, the valve I9, the valve II10 and the valve IV12 are all two-way valves, the valve III11 is a three-way valve, the front end of the valve I9 is communicated with a nitrogen gas source 8, the rear end of the valve I9 is communicated with an inlet of the permeation lower cavity 2, the front end of the valve II10 is communicated with an outlet of the permeation lower cavity 2, the rear end of the valve III11 is communicated with an end a, the c end of the valve III11 is communicated with an oxygen sensor 13, the b end of the valve III11 is suspended, and the valve IV12 is connected between the front end of.
During testing, the on-off of the pipelines from the air inlet pipeline 5, the exhaust pipeline 6 and the exhaust pipeline 6 of the lower permeation cavity to the oxygen sensor 13 is controlled by the valve I9, the valve II10, the valve III11 and the valve IV12, so that the test of the oxygen transmission rate is realized, and the specific method comprises the following steps:
s01), bypass: during the test, the valve I9 and the valve II10 are opened, the valve IV12 is closed, the ab of the valve III11 is conducted, the permeated upper cavity 1 is flowing oxygen, and the high-purity nitrogen permeated in the lower cavity 2 is exhausted from the ab of the valve III11 through the valve I9 and the valve II 10.
S02), sampling and analyzing: the ac of the valve III11 is communicated, the oxygen permeating the upper cavity 1 permeates the sample 14 to reach the lower permeating cavity 2, the nitrogen entering the lower permeating cavity 2 from the nitrogen source 8 carries the permeated oxygen to be transmitted to the oxygen sensor 13, and when the oxygen sensor 13 detects that the value of the oxygen content in the nitrogen exceeds the zero point Z0Recording the time at this time as t1After a period of time, when the oxygen content in the nitrogen gas is reduced to zero point Z0When the time is recorded as t2Simultaneously recording t1To t2Value T of staged oxygen sensorxAnd record Tx-Z0The oxygen concentration changes during this process as shown in fig. 3.
S03), starting enrichment and zero point test; closing the valve I9 and the valve II10, opening the valve IV12, keeping the valve III11 ac communicated, and forming a completely sealed chamber V1 by the valve I9, the lower permeation cavity 2 and the valve II10, wherein the sealed chamber is filled with high-purity nitrogen; the flowing high-purity nitrogen reaches the oxygen sensor 13 through the valve IV12 and the ac of the valve III11, and the oxygen sensor 13 tests the oxygen in the high-purity nitrogen, namely, the zero point test is carried out.
S04), enrichment waiting. And keeping an enrichment zero test state, under the action of the oxygen concentration difference of two sides of the sample 14, oxygen permeates from the high-concentration side to the low-concentration side of the sample 14, oxygen molecules permeating through the sample 14 are enriched in the sealed chamber V1, the oxygen content of the sealed chamber V1 is higher and higher along with the prolonging of time, and the enrichment time is determined according to the permeation rate of the sample so as to ensure that the permeated oxygen content can completely enter the effective detection range of the sensor. After the set time is reached, the process proceeds to step S02.
S05), repeating steps S02 to S04 according to S =
And calculating the value of the oxygen transmission rate until the value of S is stable, wherein S is the value of the oxygen transmission rate.
The foregoing description is only for the basic principle and the preferred embodiments of the present invention, and modifications and substitutions by those skilled in the art are included in the scope of the present invention.
Claims (2)
1. A trace oxygen transmission rate test method is characterized by comprising the following steps: the testing device for implementing the method comprises an upper permeation cavity and a lower permeation cavity, wherein the lower permeation cavity is provided with an air inlet pipeline and an air outlet pipeline, the air inlet pipeline of the lower permeation cavity is provided with a valve I, the air outlet pipeline of the lower permeation cavity is provided with a valve II and a valve III, the valve I, the valve II and the valve III are all three-way valves, the end a of the valve I is communicated with a nitrogen source, the end c of the valve I is communicated with the air inlet of the lower permeation cavity, the end c of the valve II is communicated with the air outlet of the lower permeation cavity, the end a of the valve II is communicated with the end a of the valve III, the end c of the valve III is communicated with an oxygen sensor, the end b of the valve I is communicated with the end b of;
the method comprises the following steps:
s01), the ac ends of the valve I and the valve II are communicated, the ab end of the valve III is communicated, so that an air inlet pipeline and an air outlet pipeline of the permeation lower cavity are communicated with the permeation lower cavity, the pipeline between the air outlet pipeline and the oxygen sensor is disconnected and emptied, an oxygen gas source is opened, oxygen flows in the permeation upper cavity, the nitrogen gas source is opened, and nitrogen entering the permeation lower cavity through the air inlet pipeline carries gas in the permeation lower cavity to be discharged from the air outlet pipeline;
s02), keeping the ac ends of the valve I and the valve II communicated with each other, and the ac end of the valve III communicated with each other, so that an air inlet pipeline and an exhaust pipeline of the permeation lower cavity are communicated with the permeation lower cavity, the pipeline between the exhaust pipeline and the oxygen sensor is communicated, at the moment, nitrogen entering the permeation lower cavity from a nitrogen source is transmitted to the oxygen sensor through the exhaust pipeline, the state is kept, and the value Tx-Z of the oxygen sensor is recorded0Until the oxygen sensing signal peak is completed;
s03), the ab ends of the valve I and the valve II are communicated, and the ac end of the valve III is kept communicated, so that an air inlet pipeline and an exhaust pipeline of the permeation lower cavity are disconnected with the permeation lower cavity, a completely sealed cavity V1 is formed in the permeation lower cavity, the pipelines between the exhaust pipeline and the oxygen sensor are communicated, and nitrogen in the air inlet pipeline directly enters the oxygen sensor to perform zero point test;
s04) and keeping the state of the step S03, so that oxygen molecules permeating the sample are enriched in the sealed chamber V1 to ensure that the oxygen amount permeating can completely enter the effective detection range of the oxygen sensor, and recording the zero point value of the oxygen sensor as Z0；
S05), repeat steps S02 through S04 until
The value is stable, and S is the value of oxygen transmission rate.
2. A trace oxygen transmission rate test method is characterized by comprising the following steps: the testing device for implementing the method comprises an upper permeation cavity and a lower permeation cavity, wherein the lower permeation cavity is provided with an air inlet pipeline and an exhaust pipeline, the air inlet pipeline of the lower permeation cavity is provided with a valve I, the exhaust pipeline of the lower permeation cavity is provided with a valve II and a valve III, a valve IV is arranged between the air inlet pipeline and the exhaust pipeline, the valve I, the valve II and the valve IV are all two-way valves, the valve III is a three-way valve, the front end of the valve I is communicated with a nitrogen source, the rear end of the valve I is communicated with an inlet of the lower permeation cavity, the front end of the valve II is communicated with an outlet of the lower permeation cavity, the rear end of the valve II is communicated with an a end of the valve III, a c end of the valve III is communicated with an oxygen sensor;
s01), closing the valve I and the valve II, and disconnecting the valve IV to communicate the ab end of the valve III, so that the air inlet pipeline and the air outlet pipeline of the permeation lower cavity are communicated with the permeation lower cavity, the pipeline between the air outlet pipeline and the oxygen sensor is disconnected and emptied, the oxygen source is opened to enable oxygen to flow in the permeation upper cavity, the nitrogen source is opened, and nitrogen entering the permeation lower cavity through the air inlet pipeline carries gas in the permeation lower cavity to be discharged from the air outlet pipeline;
s02), keeping the valve I and the valve II closed, and disconnecting the valve IV to connect the ac end of the valve III, so that the air inlet pipeline and the exhaust pipeline of the permeation lower cavity are communicated with the permeation lower cavity, and the exhaust pipeline is communicated with oxygenThe pipelines between the gas sensors are communicated, at the moment, nitrogen entering the permeation lower cavity from the nitrogen source is transmitted to the oxygen sensor through the exhaust pipeline, the state is maintained, and the value Tx-Z of the oxygen sensor is recorded0Until the oxygen sensing signal peak is completed;
s03), opening the valve I and the valve II, closing the valve IV, and keeping the ac end of the valve III communicated, so that an air inlet pipeline and an exhaust pipeline of the permeation lower cavity are disconnected with the permeation lower cavity, a completely sealed cavity V1 is formed in the permeation lower cavity, the pipeline between the exhaust pipeline and the oxygen sensor is conducted, nitrogen in the air inlet pipeline directly enters the oxygen sensor, and zero point test is carried out;
s04) and keeping the state of the step S03, so that oxygen molecules permeating the sample are enriched in the sealed chamber V1 to ensure that the oxygen amount permeating can completely enter the effective detection range of the oxygen sensor, and recording the zero point value of the oxygen sensor as Z0；
S05), repeat steps S02 through S04 until
The value is stable, and S is the value of oxygen transmission rate.
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| CN202486012U (en) * | 2012-03-27 | 2012-10-10 | 济南兰光机电技术有限公司 | Gas permeability test device |
| CN102928326A (en) * | 2012-11-08 | 2013-02-13 | 济南兰光机电技术有限公司 | Device and method for testing permeability of organic gases to films |
| CN104777090A (en) * | 2015-05-08 | 2015-07-15 | 广州标际包装设备有限公司 | Oxygen permeation analysis tester |
| CN205003056U (en) * | 2015-10-15 | 2016-01-27 | 济南思克测试技术有限公司 | Oxygen vapor transmissivity test all -in -one |
| CN206410980U (en) * | 2017-01-25 | 2017-08-15 | 济南思克测试技术有限公司 | A kind of gas permeation rate Auto-Test System based on artificial intelligence |
| CN108613915A (en) * | 2018-07-16 | 2018-10-02 | 济南兰光机电技术有限公司 | A kind of OTR oxygen transmission rate test device, system and method |
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