CN105929078A - Oxygen permeability test device and oxygen permeability test method - Google Patents

Oxygen permeability test device and oxygen permeability test method Download PDF

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Publication number
CN105929078A
CN105929078A CN201610408054.0A CN201610408054A CN105929078A CN 105929078 A CN105929078 A CN 105929078A CN 201610408054 A CN201610408054 A CN 201610408054A CN 105929078 A CN105929078 A CN 105929078A
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CN
China
Prior art keywords
oxygen
carrier gas
sample
cavity
gas
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Pending
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CN201610408054.0A
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Chinese (zh)
Inventor
任力
刘卅
杨军忠
王家鸣
王迎军
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Guangzhou Pudaolianxin Biotechnology Co Ltd
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Guangzhou Pudaolianxin Biotechnology Co Ltd
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Priority to CN201610408054.0A priority Critical patent/CN105929078A/en
Publication of CN105929078A publication Critical patent/CN105929078A/en
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N2030/022—Column chromatography characterised by the kind of separation mechanism
    • G01N2030/025—Gas chromatography

Abstract

The invention discloses an oxygen permeability test device and an oxygen permeability test method. The device comprises two sample clamps, an oxygen feeding device, a carrier gas feeding device and a detection device, wherein the sample clamps consist of oxygen cavities and carrier gas cavities; the oxygen cavities are connected with the oxygen feeding device through oxygen cavity feeding pipelines and are further provided with oxygen cavity discharging pipelines; the carrier gas cavities are connected with the carrier gas feeding device through carrier gas cavity feeding pipelines and are connected with the detection device through carrier gas cavity discharging pipelines; the detection device comprise a quantitative sample injection device and a gas chromatograph. The method disclosed by the invention comprises the following steps: placing a sample into the sample clamps, and feeding oxygen and carrier gas respectively to two sides of the sample. The oxygen enters the carrier gas through the sample, and the carrier gas is detected to obtain oxygen permeability data of the material. The device and the method can be used for testing the oxygen permeability of a cornea repair material; the device is long in service life, low in operation cost, small in system error and high in test precision.

Description

A kind of oxygen permeating amount test device and oxygen permeating amount method of testing
Technical field
The present invention relates to a kind of oxygen permeating amount test device and oxygen permeating amount method of testing.
Background technology
Oxygen permeability is the important performance indexes of cornea repair material, if the oxygen transmission rate of cornea repair material does not reaches requirement, Will result in cornea and be in anaerobic condition for a long time, cause corneal endothelial cell counts amount constantly to reduce, final corneal causes very Big damage, therefore, oxygen permeability detection is the important step that cornea repair material characterizes.
The detection method of common oxygen permeation of cornea repair material includes following two: 1) for contact lens,soft with artificial Cornea generally uses polarography, and sample is invested on electrode, after oxygen passes through sample and separates, occurs on the two poles of the earth of electrode Electrochemical reaction, the electric current produced by detection calculating can obtain oxygen permeating amount；2) coulomb is generally used for contact lens,hard Method, is placed in contact lense in sample clamp, and side passes to oxygen, and opposite side passes to carrier gas, and oxygen penetrates through quilt after contact lense Carrier gas is taken away, and utilizes the concentration of coulomb sensor detection oxygen.
But, all there is obvious defect in both the above method of testing: polarography can only measure contact lens,soft with artificial The oxygen permeability coefficient of cornea, applies extremely limited；Although coulomb method can be not only used for the mensuration of the oxygen permeability coefficient of contact lens,hard, it is possible to For the mensuration of the oxygen permeability coefficient of contact lens,soft, but the coulomb sensor price in coulomb method is high, and it is consumption-type device Material, maintenance maintenance frequently, uses the cycle short, and running cost is high.
The invention discloses a kind of oxygen permeating amount test device and oxygen permeating amount method of testing, to contact lens,soft, hard contact The oxygen permeating amount of mirror, artificial cornea and other cornea repair materials all can be measured, and systematic error is little, and measuring accuracy is high, operation Low cost.
Summary of the invention
It is an object of the invention to provide and the present invention relates to a kind of oxygen permeating amount test device and oxygen permeating amount method of testing.
The technical solution used in the present invention is:
A kind of oxygen permeating amount method of testing, comprises the following steps:
1) in gas chromatograph, volume V is entered1Oxygen, from spectrogram, obtain peak area S1；
2) both sides of testing sample lead to oxygen and carrier gas respectively, and the region that oxygen is exposed to oxygen stream through sample penetrates into carrier gas Side, by volume V2The mixed gas of oxygen and carrier gas send into gas chromatograph, the amount of oxygen in detection mixed gas, from spectrum Figure obtains peak area S2；
3) the oxygen permeability coefficient D of samplekCan be calculated by below equation:
Dk=(V1×S2× t × Q)/(S1×A×p×V2),
Wherein, DkFor oxygen permeability coefficient, unit is mL cm cm-2·s-1·Pa-1；V1For the volume of purity oxygen standard specimen, unit is mL；S1It it is the gas chromatogram peak area of purity oxygen standard specimen；T is the harmonic average thickness that sample is exposed to the region in oxygen stream Degree, unit is cm；Q is the flow of carrier gas, and unit is mL s-1；A is the area that sample is exposed to the region of oxygen stream, and unit is cm2；P is that sample both sides oxygen pressure is poor, and unit is Pa, and its value is equal to atmospheric pressure；V2Body for carrier gas Yu the mixed gas of oxygen Long-pending, unit is mL；S2It it is the peak area of oxygen in the mixed gas sending into gas chromatograph.
Described carrier gas is the one in nitrogen, hydrogen, helium.
A kind of oxygen permeating amount test device, including two set sample clamps, oxygen inlet duct, carrier gas inlet duct and detection dress Put；Described sample clamp is made up of oxygen chamber and carrier gas cavity；Described oxygen chamber is filled with oxygen air inlet by oxygen chamber admission line Putting connection, oxygen chamber is additionally provided with oxygen chamber outlet pipe；Described carrier gas cavity is by carrier gas cavity admission line and carrier gas inlet duct Connect, and be connected with detection device by carrier gas cavity outlet pipe；Described detection device includes quantitative sampling device and gas phase look Spectrometer.
Further, described oxygen inlet duct includes oxygen cylinder, the oxygen channel being sequentially connected with, oxygen flow regulation Valve, oxygen channelAnd oxygen flow meter.
Further, described oxygen chamber admission line is divided into two branch roads, and the oxygen chamber with two sample clamps connects respectively Connect, and be respectively equipped with oxygen air intake control valve on two branch roads.
Further, described carrier gas inlet duct includes carrier gas bottle, the carrier gas channel being sequentially connected with, carrier gas flux regulation Valve, carrier gas channelWith carrier gas flux meter.
Further, described carrier gas cavity admission line is divided into two branch roads, and the carrier gas cavity with two sample clamps connects respectively Connect, and be respectively equipped with carrier gas air intake control valve on two branch roads.
Further, described oxygen chamber is connected with the cavity wall joint screw of carrier gas cavity.
Further, the described cavity wall in oxygen chamber, the cavity wall of carrier gas cavity and sample joint are provided with sealing ring or coating is true Empty silica gel.
Further, described oxygen chamber is communicated with the external world by oxygen chamber outlet pipe.
Further, described quantitative sampling device includes six-way valve and the quantitative loop being connected, six-way valve and gas-chromatography The injection port of instrument connects.
The invention has the beneficial effects as follows:
1) device i.e. can realize the saturating of contact lens,soft, contact lens,hard, artificial cornea and other cornea repair materials Oxygen amount is tested；
2) gas chromatograph price is far below coulomb sensor, and maintenance maintenance frequency is low compared with coulomb sensor, uses the cycle remote Higher than coulomb sensor, significantly reduce running cost；
3) two sleeve clamps and path in parallel use the total amount that can improve sample introduction gas, reduce systematic error, improve test Precision, and install twin tong oxygen air intake control valve and twin tong carrier gas control valve respectively additional, beneficially mono-/bis-path switching, both Binary channel test can be realized, it is also possible to realize unipath test according to actual conditions, and can be to the stability of a system and data precision Compare.
Accompanying drawing explanation
Fig. 1 is the structural representation of the oxygen permeating amount test device of the present invention.
Fig. 2 is the structural representation of the sample clamp measuring cambered surface sample.
Fig. 3 is the structural representation of the sample clamp measuring planar sample.
Accompanying drawing indicates and illustrates: 1, oxygen channel；2, left fixture oxygen air intake control valve；3, right fixture oxygen air inlet controls Valve；4, oxygen flow rate adjusting valve；5, oxygen channel；6, oxygen flow meter；7, oxygen chamber admission line；8, oxygen chamber escape pipe Road；8A, left fixture oxygen chamber outlet pipe；8B, right fixture oxygen chamber outlet pipe；9, carrier gas channel；10, left fixture carrier gas Air intake control valve；11, right fixture carrier gas air intake control valve；12, carrier gas flux regulation valve；13, carrier gas channel；14, carrier gas flux Meter；15, carrier gas cavity admission line；16, carrier gas cavity outlet pipe；17, quantitative sampling device；18, detection installs pipes；19, gas Chromatography；20A, left sample clamp；20B, right sample clamp；21, oxygen chamber；22, sample；23, sealing ring；24, carrier gas Chamber.
Detailed description of the invention
Below in conjunction with specific embodiments and the drawings, the present invention is made further explanation and description.
Use assembly of the invention to carry out oxygen permeating amount test, comprise the following steps:
1) in gas chromatograph, volume V is entered1Oxygen, from spectrogram, obtain peak area S1；
2) both sides of testing sample lead to oxygen and carrier gas respectively, and the region that oxygen is exposed to oxygen stream through sample penetrates into carrier gas Side, by volume V2The mixed gas of oxygen and carrier gas send into gas chromatograph, the amount of oxygen in detection mixed gas, from spectrum Figure obtains peak area S2；
3) the oxygen permeability coefficient D of samplekCan be calculated by below equation:
Dk=(V1×S2× t × Q)/(S1×A×p×V2),
Wherein, DkFor oxygen permeability coefficient, unit is mL cm cm-2·s-1·Pa-1；V1For the volume of purity oxygen standard specimen, unit is mL；S1It it is the gas chromatogram peak area of purity oxygen standard specimen；T is the harmonic average thickness that sample is exposed to the region in oxygen stream Degree, unit is cm；Q is the flow of carrier gas, and unit is mL s-1；A is the area that sample is exposed to the region of oxygen stream, and unit is cm2；P is that sample both sides oxygen pressure is poor, and unit is Pa, and its value is equal to atmospheric pressure；V2Body for carrier gas Yu the mixed gas of oxygen Long-pending, unit is mL；S2It it is the peak area of oxygen in the mixed gas sending into gas chromatograph.
Preferably, the one during described carrier gas is nitrogen, hydrogen, helium.
From Fig. 1～3: the present invention oxygen permeating amount test device, including two set sample clamps (left sample clamp 20A and Right sample clamp 20B), oxygen inlet duct, carrier gas inlet duct and detection device；Described sample clamp is by oxygen chamber 21 and carries Air cavity 24 forms；Described oxygen chamber 21 is connected with oxygen inlet duct by oxygen chamber admission line 7, and oxygen chamber 21 is additionally provided with oxygen Air cavity outlet pipe 8；Described carrier gas cavity 24 is connected with carrier gas inlet duct by carrier gas cavity admission line 15, and passes through carrier gas cavity Outlet pipe 16 is connected with detection device；Described detection device is included being installed pipes by detection the quantitative sampling device of 18 connections 17 and gas chromatograph 19.
Preferably, described oxygen inlet duct includes being sequentially connected with oxygen cylinder, oxygen channel 1, oxygen flow rate adjusting valve 4, oxygen channel5 and oxygen flow meter 6.
Preferably, described oxygen chamber admission line 7 is divided into two branch roads, respectively with two sample clamp (left sample clamps 20A and right sample clamp 20B) oxygen chamber 21 connect, and on two branch roads, be respectively equipped with oxygen air intake control valve (left fixture oxygen Gas air intake control valve 2 and right fixture oxygen air intake control valve 3).
Preferably, described carrier gas inlet duct includes carrier gas bottle, the carrier gas channel being sequentially connected with9, carrier gas flux regulation valve 12, carrier gas channel13 and carrier gas flux meter 14.
Preferably, described carrier gas cavity admission line 15 is divided into two branch roads, respectively with two sample clamp (left sample clamps 20A and right sample clamp 20B) carrier gas cavity 24 connect, and be respectively equipped with on two branch roads carrier gas air intake control valve (left fixture carry Gas air intake control valve 10 and right fixture carrier gas air intake control valve 11).
Preferably, described oxygen chamber 21 is connected with the cavity wall joint screw of carrier gas cavity 24.
Preferably, the cavity wall in described oxygen chamber 21, the cavity wall of carrier gas cavity 24 and sample 22 joint be provided with sealing ring 23 or Coating vacuum silicon rubber.
Preferably, described oxygen chamber 21 is communicated with the external world by oxygen chamber outlet pipe 8.
Preferably, described quantitative sampling device 17 includes six-way valve and the quantitative loop being connected, six-way valve and gas-chromatography The injection port of instrument 19 connects.
Preferably, described six-way valve is when filling sample position, and the gaseous mixture that carrier gas cavity outlet pipe 16 flows out passes through six-way valve Entering quantitative loop, after quantitative loop is full of, unnecessary gaseous mixture is discharged from the relieving device of six-way valve；Six-way valve turns to sample introduction position Time, quantitative loop disconnects and the connection of carrier gas cavity outlet pipe 16, and connects with the vapor-phase flow path of carrier gas, and quantitative loop is rinsed in carrier gas, Promote the gaseous mixture in quantitative loop to enter gas chromatograph to be analyzed.
Preferably, described oxygen channel I1, oxygen channel II5, oxygen chamber admission line 7, oxygen chamber outlet pipe 8A, oxygen Air cavity outlet pipe 8B, carrier gas channel I9, carrier gas channel II13, carrier gas cavity admission line 15, carrier gas cavity outlet pipe 16 and inspection Survey installs pipes and 18 is tracheae.
Oxygen flow is controlled by oxygen flow rate adjusting valve 4 and is read by oxygen flow meter 6.Carrier gas flux is adjusted by carrier gas flux Joint valve 12 controls and is read by carrier gas flux meter 14.Partial oxidation can penetrate through under the effect of sample both sides oxygen concentration difference Sample 22 enters carrier gas cavity 24, and remaining oxygen is then emptied by oxygen chamber outlet pipe 8.Carrier gas channel I9, carrier gas are passed through in carrier gas Flow control valve 12, carrier gas channel II13, carrier gas flux meter 14, carrier gas cavity admission line 15 enter carrier gas cavity 24, and carrier gas is carried The oxygen penetrating through sample becomes sample gas, and quantitative sampling device is by volume V2Carrier gas and oxygen mixed gas send into gas phase Chromatograph 19, is detected the amount of oxygen in mixed gas by gas chromatograph 19.
Embodiment 1:
Test sample: the cambered surface dry state chitosan film of solid shape；
Oxygen chamber 21 is cambered surface with the cavity wall joint of carrier gas cavity 24:
Carrier gas is nitrogen；
Being respectively adopted left fixture and the test of right fixture, and contrast with coulomb method test result, test result is as shown in table 1.
Embodiment 2:
Test sample: the dry state shitosan cambered surface film of 96.7% deacetylation, oxygen chamber 21 with the cavity wall joint of carrier gas cavity 24 is Cambered surface, carrier gas is nitrogen, uses the dual channel mode test that left fixture and right fixture come into operation simultaneously, and with coulomb method test result Contrasting, test result is as shown in table 1.
Embodiment 3:
Test sample is the hygrometric state shitosan cambered surface film of 96.7% deacetylation；
Oxygen chamber 21 is cambered surface with the cavity wall joint of carrier gas cavity 24；
Carrier gas is nitrogen；
Use the dual channel mode test that left fixture and right fixture come into operation simultaneously, and contrast with coulomb method test result, survey Test result is as shown in table 1.
Embodiment 4:
Test sample: the dry state shitosan planar film of 96.7% deacetylation；
Oxygen chamber 21 is plane with the cavity wall joint of carrier gas cavity 24；
Carrier gas is nitrogen；
Use the dual channel mode test that left fixture and right fixture come into operation simultaneously, and contrast with coulomb method test result, survey Test result is as shown in table 1.
Embodiment 5:
Test sample: the hygrometric state shitosan planar film of 96.7% deacetylation；
Oxygen chamber 21 is plane with the cavity wall joint of carrier gas cavity 24；
Carrier gas is nitrogen；
Use the dual channel mode test that left fixture and right fixture come into operation simultaneously, and contrast with coulomb method test result, survey Test result is as shown in table 1.
Embodiment 6:
Test sample: the dry state shitosan cambered surface sample of collagen/96.7% deacetylation of 45% collagen content；
Oxygen chamber 21 is cambered surface with the cavity wall joint of carrier gas cavity 24；
Carrier gas is nitrogen；
Use the dual channel mode test that left fixture and right fixture come into operation simultaneously, and contrast with coulomb method test result, survey Test result is as shown in table 1.
Embodiment 7:
Test sample: the hygrometric state shitosan cambered surface sample of collagen/96.7% deacetylation of 45% collagen content；
Oxygen chamber 21 is cambered surface with the cavity wall joint of carrier gas cavity 24；
Carrier gas is nitrogen；
Use the dual channel mode test that left fixture and right fixture come into operation simultaneously, and contrast with coulomb method test result, survey Test result is as shown in table 1.
Embodiment 8:
Test sample: the shitosan planar sample of collagen/96.7% deacetylation of 45% collagen content, and with the addition of respectively quite Crosslinking agent 1-ethyl-(3-dimethyl aminopropyl) phosphinylidyne diimmonium salt hydrochlorate (EDC) in collagen 1/12,2/12；
Oxygen chamber 21 is hygrometric state planar sample with the cavity wall joint of carrier gas cavity 24；
Carrier gas is nitrogen；
Using the dual channel mode test that left fixture and right fixture come into operation simultaneously, the degree of cross linking of left and right fixture sample is different, Zuo Jia The crosslinking agent adding proportion of tool institute load sample is 1/12, and the crosslinking agent adding proportion of right fixture institute load sample is 2/12, and Contrasting with coulomb method test result, test result is as shown in table 1.
Test case:
The test result of embodiment 1～8 is as shown in table 1:
The oxygen permeability coefficient D of 1～8 implemented by table 1kTest result
Above-described embodiment is the present invention preferably embodiment, but embodiments of the present invention are not limited by above-described embodiment System, the change made, modifies, substitutes, combines, simplifies, all under other any Spirit Essence without departing from the present invention and principle Should be the substitute mode of equivalence, within being included in protection scope of the present invention.

Claims (10)

1. an oxygen permeating amount method of testing, it is characterised in that comprise the following steps:
1) in gas chromatograph, volume V is entered1Oxygen, from spectrogram, obtain peak area S1；
2) both sides of testing sample lead to oxygen and carrier gas respectively, and the region that oxygen is exposed to oxygen stream through sample penetrates into carrier gas Side, by volume V2The mixed gas of oxygen and carrier gas send into gas chromatograph, the amount of oxygen in detection mixed gas, from spectrum Figure obtains peak area S2；
3) the oxygen permeability coefficient D of samplekCan be calculated by below equation:
Dk=(V1×S2× t × Q)/(S1×A×p×V2),
Wherein, DkFor oxygen permeability coefficient, unit is mL cm cm-2·s-1·Pa-1；V1For the volume of purity oxygen standard specimen, unit is mL；S1It it is the gas chromatogram peak area of purity oxygen standard specimen；T is the harmonic average thickness that sample is exposed to the region in oxygen stream Degree, unit is cm；Q is the flow of carrier gas, and unit is mL s-1；A is the area that sample is exposed to the region of oxygen stream, and unit is cm2；P is that sample both sides oxygen pressure is poor, and unit is Pa, and its value is equal to atmospheric pressure；V2Body for carrier gas Yu the mixed gas of oxygen Long-pending, unit is mL；S2It it is the peak area of oxygen in the mixed gas sending into gas chromatograph.
2. an oxygen permeating amount test device, it is characterised in that: include two set sample clamps, oxygen inlet duct, carrier gas air inlet dress Put and detect device；Described sample clamp is made up of oxygen chamber and carrier gas cavity；Described oxygen chamber by oxygen chamber admission line with Oxygen inlet duct connects, and oxygen chamber is additionally provided with oxygen chamber outlet pipe；Described carrier gas cavity passes through carrier gas cavity admission line and load Gas inlet duct connects, and is connected with detection device by carrier gas cavity outlet pipe；Described detection device includes that quantitative sample injection fills Put and gas chromatograph.
Device the most according to claim 2, it is characterised in that: described oxygen inlet duct includes the oxygen being sequentially connected with Bottle, oxygen channel, oxygen flow rate adjusting valve, oxygen channelAnd oxygen flow meter.
Device the most according to claim 2, it is characterised in that: described oxygen chamber admission line is divided into two branch roads, respectively It is connected with the oxygen chamber of two sample clamps, and is respectively equipped with oxygen air intake control valve on two branch roads.
Device the most according to claim 2, it is characterised in that: described carrier gas inlet duct includes the carrier gas being sequentially connected with Bottle, carrier gas channel, carrier gas flux regulation valve, carrier gas channelWith carrier gas flux meter.
Device the most according to claim 2, it is characterised in that: described carrier gas cavity admission line is divided into two branch roads, respectively It is connected with the carrier gas cavity of two sample clamps, and is respectively equipped with carrier gas air intake control valve on two branch roads.
Device the most according to claim 2, it is characterised in that: described oxygen chamber and the cavity wall joint screw of carrier gas cavity Connect.
Device the most according to claim 2, it is characterised in that: state the cavity wall in oxygen chamber, the cavity wall of carrier gas cavity and sample pair The place of connecing is provided with sealing ring or coating vacuum silicon rubber.
Device the most according to claim 2, it is characterised in that: described oxygen chamber is by oxygen chamber outlet pipe and extraneous phase Logical.
Device the most according to claim 2, it is characterised in that: described quantitative sampling device includes the six-way valve being connected And quantitative loop, six-way valve is connected with the injection port of gas chromatograph.
CN201610408054.0A 2016-06-12 2016-06-12 Oxygen permeability test device and oxygen permeability test method Pending CN105929078A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109030395A (en) * 2018-07-13 2018-12-18 江苏力凡胶囊有限公司 A method of measurement Capsules oxygen transit dose

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Application publication date: 20160907