CN106546383B - Liquid refrigerant perfluoro triethylamine leakage test method - Google Patents
Liquid refrigerant perfluoro triethylamine leakage test method Download PDFInfo
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- CN106546383B CN106546383B CN201510603882.5A CN201510603882A CN106546383B CN 106546383 B CN106546383 B CN 106546383B CN 201510603882 A CN201510603882 A CN 201510603882A CN 106546383 B CN106546383 B CN 106546383B
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- perfluoro triethylamine
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- triethylamine
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Abstract
The invention discloses a kind of space products with thermally conductive coolant perfluoro triethylamine (C6F15N) the leakage test method of liquid refrigerant, utilize the effumability characteristic of liquid perfluoro triethylamine, the perfluoro triethylamine leaked in the state of unsaturation can be volatilized by blower stirring for gaseous material completely, and atmosphere level Four mass spectrum leak detection technical testing method is utilized to realize the leakage test of perfluoro triethylamine.The product that refrigeration industry uses liquid perfluoro triethylamine working medium may be implemented in test method of the invention, the practical leakage test of working medium after completing working medium filling.Leak detection is carried out compared to can more true, accurately reflection product actual leakage state using leak detection dielectric gas with existing.
Description
Technical field
The present invention relates to a kind of aerospace industries, common thermally conductive coolant perfluoro triethylamine in electron electric power industry
(C6F15N) the test method of leakage rate.In particular to the effumability characteristic for utilizing perfluoro triethylamine, using big gas chromatography-mass spectrum analysis
Principle, the method for carrying out leakage test.
Background technique
Perfluoro triethylamine is a kind of novel coolant liquid, has the inert liquid that viscosity is low, specific heat is big, non-ignitable, is boat
Its aircraft industry, common thermally conductive coolant in electron electric power industry.It is generallyd use in the Active thermal control system of spacecraft complete
Fluorine triethylamine realizes thermally conductive refrigerating function as working medium, with the continuous development of space product technology, life-time dilatation, it is desirable that
Refrigerant leakage amount in product is fewer and fewer, and leak-testing required precision is higher and higher.
The leakage test of spacecraft product at present is generally tested using probe gas, will be in product system under test (SUT)
Be filled with the consistent probe gas of operating pressure in orbit, be put into the non-real empty container of sealing, accumulate regular hour t
(generally 24 hours) measure the concentration variable quantity A1 of probe gas in closed container with instrument.Its test process belongs to phase
To measurement, after needing to demarcate test macro, the leakage rate of product just can determine that.Scaling method is to be infused using quantitative gas
Enter method to be demarcated, quantitative gas W refers to gas pressure and volume it is known that such as W=0.5MPa × 20ml.Quantitative gas W is injected
It seals in collection vessel, the concentration variable quantity A2 of probe gas in the collection vessel of quantitative gas injection front and back is measured with instrument.
Then leakage rate Q=(W/A2) × A1 of the product with respect to probe gas in the t time.Probe gas is used to carry out leakage test as state
The leak testing method of inside and outside maturation, technically reliable generally can confirm leakage of the product to probe gas before working medium filling
Amount.
It is had the following disadvantages using probe gas progress leakage test and insufficient:
1) test result is product with respect to the leakage rate of probe gas, can not directly obtain the leakage rate to working medium；
2) the actual leakage amount after product filling can not be learnt.
When the present invention proposes that space product uses liquid perfluoro triethylamine working medium, a kind of test method of refrigerant leakage amount.
Also the product that refrigeration industry uses liquid perfluoro triethylamine working medium may be implemented, the practical leakage of working medium after completing working medium filling
Measure examination.
Summary of the invention
The object of the present invention is to provide a kind of leakage test methods of liquid refrigerant perfluoro triethylamine.
To achieve the goals above, present invention employs the following technical solutions:
A kind of leakage test method of space product liquid refrigerant perfluoro triethylamine utilizes liquid perfluor three
The effumability of ethamine, it is gaseous material that the perfluoro triethylamine leaked under unsaturated state, which stirs volatilization completely by blower,
The mass spectrometric analysis method of gas is recycled to carry out leakage test.
Wherein, the leakage test of perfluoro triethylamine is carried out using the level Four mass spectrum leak detection analysis method of atmosphere.
Wherein, the structural formula of perfluoro triethylamine are as follows:
Wherein, the spectral peak of perfluoro triethylamine is 119 (CF3CF2)+With 69 (CF3)+。
Wherein, the method specifically comprises the following steps:
1) test product is filled into liquid refrigerant perfluoro triethylamine to authorized pressure；
2) test product is placed in closed container, keeps predetermined time t, is stirred with blower, make the liquid of leakage
State working medium is volatilized completely and is uniformly mixed with atmosphere, and closed container is non-real empty container, and sealing performance index is in internal pressure
Under 2kPa, leakage in 24 hours is not more than 150Pa；
3) with the concentration increments A1 of the spectral peak 119 and 69 of perfluoro triethylamine in quadruple mass-spectrometer test closed container；
4) microsyringe is recycled, precision 2% takes the perfluoro triethylamine liquid refrigerant of Wml；
5) taken liquid is refilled in closed container, is stirred with blower, make leak working medium volatilize completely and
It is uniformly mixed with atmosphere；
6) again with the further increment of concentration of liquid refrigerant spectral peak 119 and 69 in quadruple mass-spectrometer test closed container
A2 completes system calibrating；
7) the leakage rate Q, Q=W × A1/A2 of product t time are calculated using following formula.
Wherein, sampling amount W is usually a certain determination value within the scope of 0.1ml~1ml.
Wherein, predetermined time t is usually at 24 hours or more.
The leakage test method of liquid refrigerant perfluoro triethylamine proposed by the present invention, can direct test product servicing fluids
After state working medium, the leakage rate of opposite liquid refrigerant t time, the slip during really reflecting product in orbit is effectively avoided
The deviation generated using leak detection dielectric tests leak rate, improves the accuracy of test.
Detailed description of the invention
Fig. 1 is the structural schematic diagram for implementing liquid refrigerant perfluoro triethylamine leakage test method of the invention.
Wherein, 1 is gas circulator；2 be quadruple mass-spectrometer；3 be test pipeline；4 be stirring blower；5 be closed container；
6 be microsyringe；7 be test product.
Specific embodiment
Introduced below is the specific embodiment as content of the present invention, below by specific embodiment to this
The content work of invention further illustrates.Certainly, description following detailed description is only example not Tongfang of the invention
The content in face but should not be understood as the limitation scope of the invention.
Fig. 1 shows the structural schematic diagram for implementing liquid refrigerant perfluoro triethylamine leakage test method of the invention.It will
Test product 7 be arranged in closed container 5, in closed container 5 setting stirring blower 4, quadruple mass-spectrometer by test pipeline 3 with
Closed container 5 is connected to, and testing tube road is provided with gas circulator 1, and microsyringe 6 may be provided at the side of closed container 5
On.
Gas circulator 1 mainly realizes that gas recycles in test pipeline 3 and sealing container 5, guarantees that gas componant is uniform, one
As choose flow be 1NL/min circulating pump, can satisfy test request.
Quadruple mass-spectrometer 2 is the core equipment of liquid refrigerant perfluoro triethylamine leakage test, due to perfluoro triethylamine two
A main spectral peak is respectively 119 and 69, needs quadruple mass-spectrometer that can test mass number range not less than 200, to perfluoro triethylamine
The resolution ratio of concentration determination is better than 0.1ppm.
Test pipeline 3 is mainly used to extract minimum gas out of sealing container, by quadruple mass-spectrometer 2 come to gas componant
It is analyzed.
Stirring blower 4 is mainly used to make the liquid of sealing container internal leakage quickly to volatilize and be uniformly mixed with atmosphere, stirs
The air output of blower requires the air circulation in 5 minutes in sealing container primary.
Sealing container 5 is mainly used to collect the liquid of leakage, is non-real empty container, and the volume energy of sealing container contains tested
Product, for sealing performance index at internal pressure 2kPa, leakage in 24 hours is not more than 150Pa.
Microsyringe 6 is mainly used to take the perfluoro triethylamine of certain volume, selects specification for 1ml, precision 2%.It send specially
Industry metrological service is sampled volume accuracy calibration.
Test product 7 needs to have the ability for bearing design pressure by pressure testing.
Wherein, test product is usually space product, uses perfluoro triethylamine as thermally conductive coolant, perfluoro triethylamine
Saturated vapour pressure is about 14900Pa, about 17300Pa at a temperature of 25 DEG C at a temperature of lower 20 DEG C of normal pressure.According to formulaAt 20 DEG C of room temperature, 100m3It can be reachable with perfluoro triethylamine quality existing for gaseous state in sealing container
226kg, according to the pure perfluoro triethylamine density 1.708g/cm of liquid3Calculating corresponding volume is 130l.Spacecraft is leaked and is surveyed
General magnitude is tried at ml grades.
The leakage test of perfluoro triethylamine is realized using atmosphere level Four mass spectrum leak detection technical testing method.
Using above-mentioned liquid refrigerant perfluoro triethylamine leakage test method, include the following steps:
1) product is filled into liquid refrigerant perfluoro triethylamine to authorized pressure by design requirement by check system；
2) product is placed in closed container, keeps predetermined time 26h, is stirred stipulated time 20min with blower,
Leakage working medium is set to volatilize and be uniformly mixed completely with atmosphere；
3) with the concentration increments A1 of the spectral peak 119 and 69 of perfluoro triethylamine in quadruple mass-spectrometer test closed container；
4) microsyringe is utilized, precision 2% takes the pure solution of the perfluoro triethylamine of 0.3ml；
5) taken liquid is injected in sealing container, is stirred stipulated time 20min with blower, keep leakage working medium complete
It volatilizees and is uniformly mixed with atmosphere；
6) the further increment A2 of concentration of perfluoro triethylamine spectral peak 119 and 69 in closed container is tested with quadruple mass-spectrometer,
Complete system calibrating；
7) the leakage rate Q, Q=W × A1/A2 of product t time are calculated using following formula.
Although the detailed description and description of the specific embodiments of the present invention are given above, it should be noted that
We can carry out various equivalent changes and modification to above embodiment according to the concept of the present invention, and generated function is made
It, should all be within protection scope of the present invention when with the spirit still covered without departing from specification and attached drawing.
Claims (5)
1. the leakage test method of space product liquid refrigerant perfluoro triethylamine utilizes liquid perfluoro triethylamine
Effumability, it is gaseous material that the perfluoro triethylamine leaked under unsaturated state, which stirs volatilization completely by blower, is recycled
The mass spectrometric analysis method of gas carries out leakage test, wherein the method specifically comprises the following steps:
1) test product is filled into liquid refrigerant perfluoro triethylamine to authorized pressure；
2) test product is placed in closed container, keeps predetermined time t, is stirred with blower, make the liquid work of leakage
Matter is volatilized completely and is uniformly mixed with atmosphere, and closed container is non-real empty container, and sealing performance index is in internal pressure 2kPa
Under, leakage in 24 hours is not more than 150Pa；
3) with the concentration increments A1 of the spectral peak 119 and 69 of perfluoro triethylamine in quadruple mass-spectrometer test closed container；
4) recycle microsyringe, precision 2% takes the perfluoro triethylamine liquid refrigerant of Wml, sampling amount W be 0.1ml~
A certain determining value within the scope of 1ml；
5) taken liquid is refilled in closed container, is stirred with blower, make leak working medium volatilize completely and with it is big
Gas is uniformly mixed；
6) complete again with the concentration further increment A2 of liquid refrigerant spectral peak 119 and 69 in quadruple mass-spectrometer test closed container
At system calibrating；
7) product is calculated in the leakage rate Q, Q=W × A1/A2 of t time using following formula.
2. leakage test method as described in claim 1, wherein carried out using the level Four mass spectrum leak detection analysis method of atmosphere
The leakage test of perfluoro triethylamine.
3. leakage test method as claimed in claim 1 or 2, wherein the structural formula of perfluoro triethylamine are as follows:
4. leakage test method as described 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 or 2, wherein the t time was at 24 hours or more.
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| CN108195524B (en) * | 2017-12-06 | 2021-02-09 | 北京航天控制仪器研究所 | Oil leakage rate detection process 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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| WO2006093935A2 (en) * | 2005-02-28 | 2006-09-08 | Advanced Technology Materials, Inc. | Apparatus and process for leak-testing and qualification of fluid dispensing vessels |
| WO2009136037A2 (en) * | 2008-04-03 | 2009-11-12 | Alcatel Lucent | Method and device for testing a container for leaks |
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