CN106546383A - Liquid refrigerant perfluoro triethylamine leakage test method - Google Patents

Liquid refrigerant perfluoro triethylamine leakage test method Download PDF

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Publication number
CN106546383A
CN106546383A CN201510603882.5A CN201510603882A CN106546383A CN 106546383 A CN106546383 A CN 106546383A CN 201510603882 A CN201510603882 A CN 201510603882A CN 106546383 A CN106546383 A CN 106546383A
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China
Prior art keywords
leakage
perfluoro triethylamine
leakage test
liquid refrigerant
test method
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CN201510603882.5A
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CN106546383B (en
Inventor
师立侠
刘胜
窦仁超
冯琪
洪晓鹏
任国华
韩琰
刘兴悦
杨定魁
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Beijing Institute of Spacecraft Environment Engineering
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Beijing Institute of Spacecraft Environment Engineering
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Abstract

The invention discloses a kind of space product heat conduction coolant perfluoro triethylamine (C6F15N) the leakage test method of liquid refrigerant, using the effumability characteristic of liquid perfluoro triethylamine, the perfluoro triethylamine leaked in the state of unsaturation can be volatilized for gaseous material completely by blower fan stirring, realize the leakage test of perfluoro triethylamine using air level Four mass spectrum leak detection technical testing method.The method of testing of the present invention can realize product of the refrigeration industry using liquid perfluoro triethylamine working medium, the actual leakage test of working medium after working medium filling is completed.The actual leakage state of product can be reflected compared with existing employing leak detection dielectric gas is hunted leak more true, exactly.

Description

Liquid refrigerant perfluoro triethylamine leakage test method
Technical field
The present invention relates to a kind of aerospace industries, the heat conduction coolant commonly used in electron electric power industry Perfluoro triethylamine (C6F15N) the method for testing of leakage rate.More particularly to using the easy of perfluoro triethylamine Volatile nature, using big gas chromatography-mass spectrum analysis principle, the method for carrying out leakage test.
Background technology
Perfluoro triethylamine is a kind of new coolant, with viscosity is low, specific heat big, do not fire it is nontoxic Inert fluid, is aerospace industries, conventional heat conduction coolant in electron electric power industry.In boat Generally adopt perfluoro triethylamine in the Active thermal control system of its device as working medium to realize heat conduction cooling work( Can, with the continuous development of space product technology, life-time dilatation, it is desirable to which the working medium in product is let out Leakage quantity is fewer and feweri, leak-testing required precision more and more higher.
The leakage test of spacecraft product, is typically tested using probe gas at present, will be produced The probe gas consistent with operating pressure in orbit is filled with product system under test (SUT), a sealing is put into In non-real empty, regular hour t (generally 24 hours) is accumulated, is measured with instrument closed Concentration change amount A1 of probe gas in container.Its test process belongs to relative measurement, needs to surveying After test system is demarcated, the leakage rate of product is just can determine that.Scaling method is to adopt quantitative gas Injection method is demarcated, quantitative gas W refer to gas pressure and volume, it is known that as W=0.5MPa × 20ml.By in quantitative gas W injection sealing collection vessels, quantitative gas injection is measured with instrument In front and back in collection vessel probe gas concentration change amount A2.Then in the t times, product is relative shows gas leakage Leakage rate Q=(the W/A2) × A1 of body.It is domestic and international to adopt probe gas to carry out leakage test Ripe leak testing method, technically reliable typically can confirm product to showing before working medium filling The leakage rate of gas leakage body.
Leakage test is carried out using probe gas to suffer from the drawback that and not enough:
1) test result is leakage rate of the product with respect to probe gas, it is impossible to directly obtained to working medium Leakage rate;
2) cannot learn that product fills the actual leakage amount after terminating.
When the present invention proposes that space product adopts liquid perfluoro triethylamine working medium, a kind of refrigerant leakage amount Method of testing.Product of the refrigeration industry using liquid perfluoro triethylamine working medium can also be realized, Complete the actual leakage test of working medium after working medium is filled.
The content of the invention
It is an object of the invention to provide a kind of leakage test method of liquid refrigerant perfluoro triethylamine.
To achieve these goals, present invention employs following technical scheme:
A kind of leakage test method of space product with liquid refrigerant perfluoro triethylamine, which utilizes liquid The effumability of state material perfluoro triethylamine, the perfluoro triethylamine leaked under unsaturation state pass through Blower fan stirring volatilization completely is gaseous material, recycles the mass spectrometric analysis method of gas to carry out leakage rate Test.
Wherein, the leakage rate of perfluoro triethylamine is carried out using the level Four mass spectrum leak detection analysis method of air Test.
Wherein, the structural formula of perfluoro triethylamine is:
Wherein, the spectral peak of perfluoro triethylamine is 119 (CF3CF2)+With 69 (CF3)+
Wherein, methods described specifically includes following steps:
1) test product is filled into liquid refrigerant perfluoro triethylamine to authorized pressure;
2) test product is placed in hermetic container, keeps scheduled time t, stirred with blower fan Mix, the liquid refrigerant of leakage is volatilized completely and is mixed homogeneously with air, hermetic container is non-real Empty, internally under pressure 2kPa, the leakage of 24 hours is not more than 150Pa to sealing property index;
3) with quadruple mass-spectrometer test hermetic container in perfluoro triethylamine spectral peak 119 and 69 it is dense Degree increment A1;
4) microsyringe is recycled, precision is 2%, takes the perfluoro triethylamine liquid refrigerant of Wml;
5) taken liquid is refilled in hermetic container, is stirred with blower fan, make leakage working medium Volatilize completely and mix homogeneously with air;
6) again with quadruple mass-spectrometer test hermetic container in liquid refrigerant spectral peak 119 and 69 it is dense Further increment A2 is spent, completion system is demarcated;
7) leakage rate Q of product t times, Q=W × A1/A2 are calculated using below equation.
Wherein, sampling amount W is usually a certain determination value in the range of 0.1ml~1ml.
Wherein, scheduled time t is generally more than 24 hours.
The leakage test method of liquid refrigerant perfluoro triethylamine proposed by the present invention, directly can survey After trial product filling liquid refrigerant, with respect to the leakage rate of liquid refrigerant t times, truly reflect product Slip during in orbit, effectively prevent the deviation produced using leak detection dielectric tests leak rate, Improve the accuracy of test.
Description of the drawings
Fig. 1 is that the structure of the liquid refrigerant perfluoro triethylamine leakage test method for implementing the present invention is shown It is intended to.
Wherein, 1 is gas circulator;2 is quadruple mass-spectrometer;3 are test pipeline;4 are stirring wind Machine;5 is hermetic container;6 is microsyringe;7 is test product.
Specific embodiment
Introduced below is the specific embodiment as content of the present invention, below by concrete Embodiment is further illustrated to the content of the present invention.Certainly, following concrete reality is described The content for only for example different aspect of the invention applying mode, and should not be construed as limiting the invention model Enclose.
Fig. 1 shows the knot of the liquid refrigerant perfluoro triethylamine leakage test method for implementing the present invention Structure schematic diagram.Test product 7 is arranged in hermetic container 5, stirring is set in hermetic container 5 Blower fan 4, quadruple mass-spectrometer are connected with hermetic container 5 by testing pipeline 3, are arranged on test pipeline There is gas circulator 1, microsyringe 6 is may be provided on the side of hermetic container 5.
Gas circulator 1 is main to realize test pipeline 3 with gas circulation in sealing container 5, it is ensured that Gas componant is uniform, the general circulating pump for choosing flow for 1NL/min, can meet test request.
Nucleus equipment of the quadruple mass-spectrometer 2 for liquid refrigerant perfluoro triethylamine leakage test, due to The main spectral peak of perfluoro triethylamine two is respectively 119 and 69, needs quadruple mass-spectrometer energy test quality Number scope is not less than 200, is better than 0.1ppm to the resolution of perfluoro triethylamine concentration determination.
Test pipeline 3 is mainly used to minimum gas are extracted from sealing container, by quadruple mass-spectrometer 2 To be analyzed to gas componant.
Stirring blower fan 4 is mainly used to make the liquid of sealing container internal leakage quickly volatilize and mixed with air Close uniform, the air circulation in air output 5 minutes interior sealing containers of requirement of stirring blower fan is once.
Sealing container 5 is mainly used to the liquid for collecting leakage, is non-real empty, sealing container Volume energy contains test product, and sealing property index is internally under pressure 2kPa, the leakage of 24 hours No more than 150Pa.
Microsyringe 6 is mainly used to the perfluoro triethylamine for taking certain volume, and selection specification is 1ml, Precision 2%.Professional metrological service is sent to be sampled volume accuracy calibration.
Test product 7 is needed through pressure test, with the ability for bearing design pressure.
Wherein, test product is typically space product, and which adopts perfluoro triethylamine to cool down as heat conduction Agent, at a temperature of perfluoro triethylamine normal pressure is lower 20 DEG C, saturated vapour pressure is about 14900Pa, 25 DEG C of temperature It is about down 17300Pa.According to formulaIn 20 DEG C of room temperature, 100m3Sealing container It is interior can with gaseous state exist perfluoro triethylamine quality up to 226kg, it is close according to the pure perfluoro triethylamine of liquid Degree 1.708g/cm3Corresponding volume is calculated for 130l.For the general magnitude of spacecraft leak-testing exists Ml levels.
Realize that using air level Four mass spectrum leak detection technical testing method the leakage of perfluoro triethylamine is measured Examination.
Using above-mentioned liquid refrigerant perfluoro triethylamine leakage test method, comprise the steps:
1) product is extremely specified by design requirement filling liquid refrigerant perfluoro triethylamine by check system Pressure;
2) product is placed in hermetic container, keeps scheduled time 26h, stirred with blower fan Stipulated time 20min is mixed, leakage working medium is volatilized completely and is mixed homogeneously with air;
3) spectral peak 119 and 69 of perfluoro triethylamine in hermetic container is tested with quadruple mass-spectrometer Concentration increments A1;
4) microsyringe is utilized, precision is 2%, takes the pure solution of perfluoro triethylamine of 0.3ml;
5) taken liquid is injected in sealing container, stipulated time 20min is stirred with blower fan, Leakage working medium is made to volatilize completely and mix homogeneously with air;
6) with quadruple mass-spectrometer test hermetic container in perfluoro triethylamine spectral peak 119 and 69 it is dense Further increment A2 is spent, completion system is demarcated;
7) leakage rate Q of product t times, Q=W × A1/A2 are calculated using below equation.
Although giving detailed description above to the specific embodiment of the present invention and illustrating, should This is intended that we can carry out various equivalent according to the conception of the present invention to above-mentioned embodiment Change and change, the spirit still covered without departing from description and accompanying drawing by the function produced by which When, all should be within protection scope of the present invention.

Claims (7)

1. leakage test method of a kind of space product with liquid refrigerant perfluoro triethylamine, which utilizes liquid The effumability of material perfluoro triethylamine, the perfluoro triethylamine leaked under unsaturation state pass through wind Machine stirring volatilization completely is gaseous material, recycles the mass spectrometric analysis method of gas to carry out leakage measurement Examination.
2. leakage test method as claimed in claim 1, wherein, examined using the level Four mass spectrum of air Leakage analysis method carries out the leakage test of perfluoro triethylamine.
3. leakage test method as claimed in claim 1 or 2, wherein, the structure of perfluoro triethylamine Formula is:
4. leakage test method as claimed in claim 1, wherein, the spectral peak of perfluoro triethylamine is 119 (CF3CF2)+With 69 (CF3)+
5. leakage test method as claimed in claim 1, wherein, methods described specifically includes as follows Step:
1) test product is filled into liquid refrigerant perfluoro triethylamine to authorized pressure;
2) test product is placed in hermetic container, keeps scheduled time t, carried out with blower fan Stirring, makes the liquid refrigerant of leakage volatilize completely and mix homogeneously with air, and hermetic container is non- Dewar vessel, internally under pressure 2kPa, the leakage of 24 hours is not more than sealing property index 150Pa;
3) spectral peak 119 and 69 of perfluoro triethylamine in hermetic container is tested with quadruple mass-spectrometer Concentration increments A1;
4) microsyringe is recycled, precision is 2%, takes the perfluoro triethylamine liquid refrigerant of Wml;
5) taken liquid is refilled in hermetic container, is stirred with blower fan, make leakage work Matter is volatilized completely and is mixed homogeneously with air;
6) liquid refrigerant spectral peak 119 and 69 in hermetic container is tested with quadruple mass-spectrometer again The further increment A2 of concentration, completion system are demarcated;
7) leakage rate Q of product t times, Q=W × A1/A2 are calculated using below equation.
6. leakage test method as claimed in claim 5, wherein, sampling amount W be usually 0.1ml~ A certain determination value in the range of 1ml.
7. leakage test method as claimed in claim 1 or 2, wherein, the scheduled time, t generally existed More than 24 hours.
CN201510603882.5A 2015-09-21 2015-09-21 Liquid refrigerant perfluoro triethylamine leakage test method Active CN106546383B (en)

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Cited By (2)

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CN108195524A (en) * 2017-12-06 2018-06-22 北京航天控制仪器研究所 A kind of oil spill rate characterization processes method
CN109541102A (en) * 2018-11-20 2019-03-29 中广核研究院有限公司 A kind of device and method of volatile organic matter vapour pressure measurement

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