1、Designation: D4991 07 (Reapproved 2015)Standard Test Method forLeakage Testing of Empty Rigid Containers by VacuumMethod1This standard is issued under the fixed designation D4991; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the
2、 year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the testing of empty containersfor resistance to leakage under differential pressure
3、conditionssuch as those which can occur during air transport. It is suitablefor testing rigid containers intended for the transportation ofsome hazardous liquids in accordance with the United NationsRecommendations On The Transport Of Dangerous Goods(UN TDG) and the International Civil Aviation Orga
4、nizationTechnical Instructions For The Safe Transport Of DangerousGoods By Air (ICAO TIs).1.2 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practic
5、es and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D996 Terminology of Packaging and Distribution Environ-mentsD3078 Test Method for Determination of Leaks in FlexiblePackaging by Bubble Emission2.2 United Nations Document:ST/SG/AC.1
6、0/1 Recommendations On The Transport OfDangerous Goods32.3 International Civil Aviation Organization:DOC 9284-AN/905 Technical Instructions For The SafeTransport Of Dangerous Goods By Air43. Terminology3.1 Definitions: Terms and definitions used in this testmethod may be found in Terminology D996.3.
7、2 Definitions of Terms Specific to This Standard:3.2.1 rigid containera container sufficiently rigid thatunder a positive pressure of 100-kPa gage the volumetricexpansion does not exceed 0.5 %, such as a glass bottle.4. Summary of Test Method4.1 An empty rigid container to be tested is pressurized b
8、yimmersion in an ethylene glycol-water solution in a transparenttest chamber and subjected to a gradually increasing partialvacuum. The container is observed for signs of leakage, asevidenced by escaping air bubbles during depressurization orfluid in the container after re-pressurization.5. Signific
9、ance and Use5.1 Containers may be pressurized in accordance with thistest method without modification to the closure or to the bodyof the container. This test method may be used for testing rigidcontainers intended for the transportation of some liquids by airin accordance with the ICAO TIs or in ac
10、cordance with the UNTDG.5.2 This test method establishes the point at which leakagecommences, with a limit of approximately 95-kPa (13.8-psi)differential. See Test Method D3078 for flexible packages.5.3 This test method may not be suitable for some packages,such as packages with paper cap seals, whe
11、re the test fluid mayrapidly deteriorate the packaging.6. Apparatus6.1 Transparent Vessel, large enough to permit the testspecimen(s) to be immersed in the test fluid with a minimumheadspace of 20 %, capable of withstanding at least 112-atmpressure differential, fitted with a flat vacuum-tight cover
12、 isrequired.6.2 Vacuum Gage, Inlet Tube from a Source of Vacuum, andOutlet Tube to the Atmosphere, shall be sealed into the cover.The inlet and outlet tubes shall be equipped with handoperatedvalves. The vacuum gage shall be laboratory quality with afull-scale range from 0 to 100 kPa (0 to 14.5 psi)
13、 with1This test method is under the jurisdiction of ASTM Committee D10 onPackaging and is the direct responsibility of Subcommittee D10.21 on ShippingContainers and Systems - Application of Performance Test Methods.Current edition approved May 1, 2015. Published July 2015. Originally approvedin 1994
14、. Last previous edition approved in 2007 as D4991 07. DOI: 10.1520/D4991-07R15.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page o
15、nthe ASTM website.3Available from United Nations Sales Section, United Nations, New York, NY10017.4Available from Intereg Group, Inc., 5724 N. Pulaski Rd., Chicago, IL 60646.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1minimum grad
16、uations no greater than 2 kPa (0.3 psi) andaccuracy to within 1 %. A suitable moisture trap, to preventback-flow of liquid, should be fitted between the vacuum gageand the source of vacuum.6.3 Solution of Ethylene Glycol in Water, 50 % by Volumefor use as a test fluid, at ambient temperature unless
17、otherwisespecified, is required. Where a test temperature other thanambient is specified, the solution shall be at the specified testtemperature. Other solutions may be required for high and lowtemperatures.NOTE 1If ethylene glycol antifreeze solution is used, it should beclarified by filtering thro
18、ugh activated charcoal.6.4 A suitable means to hold the test specimen(s) with theclosure(s) not more than 25 mm (1 in.) under the surface of thetest fluid is required. The method of restraint should not affectthe results of the test.7. Test Specimens7.1 Test specimens shall consist of containers, in
19、cludingtheir closures. Test specimens of containers which are inproduction shall be representative samples, taken at random.7.2 Containers shall be empty containers which previouslycontained any substance and were cleaned of the contents priorto testing. New containers and closures, where available,
20、should be used.7.3 Each container shall be closed for testing in the samemanner as it would be closed for actual shipment. All closuresshall be installed using the techniques or torques specified bythe closure manufacturer, container manufacturer, or shipper.Close containers at ambient pressure and
21、temperature.7.4 Where a test temperature other than ambient is specified,the sample containers shall be conditioned at the test tempera-ture for at least 24 h, and until they reach equilibrium oftemperature with the conditioning atmosphere.7.5 Unless otherwise specified, test at least three specimen
22、s.8. Preparation of Apparatus8.1 Assemble the apparatus in accordance with Fig. 1.8.2 Prior to testing, draw a vacuum to at least 95-kPa(13.8-psi) differential and maintain this vacuum for 10 min inorder to remove air dissolved in the test fluid.9. Procedure9.1 Immerse the test specimens in the ethy
23、lene glycol-watersolution inside the transparent test chamber. Remove as manybubbles as possible from the outer surface of the test specimensby agitation or other means.9.1.1 More than one specimen can be tested at one timeprovided that there is sufficient space in the test chamber toallow clear obs
24、ervation of each specimen. If this is done, affixthe test specimens so closures are sufficiently separated topermit individual observation of each, to detect leakage.9.2 Seal the lid, open the hand valve on the inlet tube, andclose the hand valve on the outlet tube to the atmosphere. Turnon the vacu
25、um so that the gage rises slowly (from 30 s to 1min) to a pressure differential of 95 kPa (13.8 psi), or otherspecified pressure differential. The vacuum can be controlledby cracking open the hand valve on the outlet tube. During therise in vacuum, observe the test specimen(s) for leakage asevidence
26、d by a continuous stream or recurring succession ofsmall bubbles. Isolated bubbles caused by trapped air are notconsidered evidence of leakage. Maintain the vacuum for aminimum of 10 min. For test specimens which are singlepackagings or combination packagings in whole or part ofplastic material, mai
27、ntain the vacuum for 30 min. Then turn thevacuum off and release it slowly by opening the hand valve onthe outlet tube. Keep the test specimen(s) immersed for at least30 s at ambient pressure. Remove the test specimen(s) andexamine the inside for fluid.9.3 Leakage is indicated by a continuous stream
28、 or recurringsuccession of bubbles. Fluid within the test specimen is alsoevidence of leakage.10. Report10.1 Report the following information:10.1.1 Identification of the containers and closures, usingmanufacturers part numbers and descriptions or using ex-ploded view drawings or cross-sectional dra
29、wings, includingdetailed data on material construction,10.1.2 Total number of specimens tested,10.1.3 Number of specimens tested at one time,10.1.4 Test pressure requirement, where applicable,10.1.5 Whether test was performed at ambient temperatureand if not, the test temperature. If a test solution
30、 other than50 % ethylene glycol was used, identify the solution,10.1.6 Whether test specimens passed or failed the test,where applicable,10.1.7 Whether each test specimen leaked and at whatpressure differential,10.1.8 Whether test fluid was apparent in each test specimenafter testing,10.1.9 A statem
31、ent to the effect that all tests were made infull compliance with the requirements of this test method, ornoting any variations and detailing them, andFIG. 1 Typical Test Setup for Leakage Testing of Containers byVacuum MethodD4991 07 (2015)210.1.10 The name and address of the testing agency, thedat
32、e, and the signature of a responsible representative of thetesting agency.11. Precision and Bias11.1 No information is presented about either the precisionor bias of this test method for measuring leaking of rigid plasticcontainers since the result is non-quantitative. It is recom-mended that test s
33、ensitivities be determined and a positive andnegative control be used when validating the test method.11.2 Once validated, the user does not have to apply thepositive and negative controls before each test.12. Keywords12.1 containers; leakage testing; packaging; vacuummethodAPPENDIX(Nonmandatory Inf
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39、0; http:/ X1.1 Pressure Conversion TablePressureDifferentialAKiloPascalsPounds per squareinch (psi)Inches of mercuryin Hg (20C)Bar10 1.45 2.96 0.1020 2.90 5.93 0.2030 4.35 8.89 0.3040 5.80 11.85 0.4050 7.25 14.82 0.5060 8.70 17.78 0.6070 10.15 20.75 0.7075 10.88 22.23 0.7580 11.60 23.71 0.8085 12.33 25.19 0.8590 13.05 26.67 0.9095 13.78 28.16 0.95100 14.50 29.64 1.00101.325 14.70 30.03 1.01325Apsi 6.894757 = kPain. Hg 3.37411 = kPabar 100 = kPaD4991 07 (2015)3
