Bescoomen 5 Tueratoal Saba; Guies and Reveanscedahns isd 9s he Wor ude rsa Teck Bans to ae cD Conn Aly Designation: D3078 - 02 (Reapproved 2021)" Standard Test Method for Determination of Leaks in Flexible Packaging by Bubble Emission" hic sun uur he Aiden DI07%; the nanber imme fling the designation egal spon in th eat of eeision the yea of fst vison A sumer in orth ios J es the yer ot st teapgeval A Spovscipt ese (c ndeas an eral chango sage te Ls Fevison ce FepPOval NOTE —Reywonts wow ade eerily Jarry 2021 1. Seope 1.1 This test method covers the determination of goss leaks in flexible packaging containing a headspace gas, Test sensi- tivity is fimited to Tx 10-° am em’ (1 x 10-* Pam) or even less sensitive as indicated in a recent interlaboratory test (eepomted in Section 12) 1.2 Small leaks may not be detected by this. procedure. -oelustic effecis on the products, or entrapped air, become significant and prevent passage through small openings. Posi- tive pressure inside the pouch after the vacuum is drawn may force the product to plug small leaks. The size of the leak that ccan be detected is dependent upon the products contained, the nature of the packaging material, and the test parameters selected 1.3 The values stated in inch-pound units are to be regarded 4s standard. The values given in parentheses are mathematical conversions t0 SI units that are provided for information only and are not considered standard 4 This standard does not purport 10 address all of the safely concerns, if any. associaed with its use. Te is the responsiblity of the user of this standard 10 establish appro- priate safety, health, and environmental practices and dever- ‘mine the applicability of regulatory limitations prior to use. LS This international standard was developed in accor dance with internationally recognized prineiples on standard ication established in the Decision on Principles for the Deselopment of International Standards, Guides and Recor ‘mendations issued by the World Traile Organization Technical Barriers 10 Trade (TBT) Comauidce, “Thiet etd sue the jisicon of ASTM Commitee FOR en Prinasy Sankey Packigag and Se det esp of Subcom es 702.4 on Package ine Cites eon apne So. (3, 2021 Pa Febasry 2021, Ong syed PTE La ea cain agreed 4 2019» B78 02 2. Referenced Documents 2. ASTI Standards? 125 Definitions of Terms Relating to Leak Testing (With- drawn 1991 FSIS Practice for Leaks Using Bubble Emission Techniques FOS Recommended Practice for Determining Hermetcity of econ Devices by a Bubble Test (Withdrawn 1984)* 3. Terminology 341 Definitions: 3.1.1 Jeak—any opening in a exible package that, comusary to intention, ether allows the contents to escape or Substances to enter, 4, Apparatus 4.1 Vacwon Chamber—Any wansparent container capable ‘of withstanding approximately one almosphere pressure differential, ited with a vacuum-tight cover. A vacuum gauge, fan inlet tube from a source of vacuum, and an outlet tube to the atmosphere shall be connected to the chamber cover. The inlet and outles tibes shall be equipped with hand valves. Attached to the underside of the cover shall be a transparent plate that will closely approximate the inside dimensions of the container ‘and be such a distance fren the top of the container that when it is two-thirds filled with Buid, the attached plate will be positioned 1 in. (25 mm) under the fui, 5. Materials Sl Inimersion Fluids—Use an immersion fluid which docs not degrade the package being tested. Fluids with a low surface 2 Far refrenend ASTM stunda,vs the ASTM web, wonnasmerg ‘emai ASTM Casomer Service aves ang Fur Aa! Bool AST Stents volume iafnaton rk lo he ans Docunet Sihay agec Ue ASTM website ‘The Mik appONEL yenlon of WS NST SAMY IS eerese wens. ‘ioyc OAS lasers 1 Rar Hae Ors, PO BCP. Wet Cnr, PARES Und Stes Ify 03078 — 02 (2021)** tension are generally more sensitive, Examples include water, ‘water treated with a weusing agent, denatured alcohol, and ‘mineral oil. Other possible Aluids ave listed in Practice E515 and Recommended Practice F98. 6, Sampling 6.1 The number of specimens used in the test sample may be varied according to the nature of the product, its cost, its size, and whether the specimens are taken from & production line in a normal packaging operation, or ane few in number, or are to be used only for purposes of comparative evaluation of procedures or materials 7. Test Specimen 7.1 Flexible Package, with or without its intended contents. 8. Conditioning 8.1 The test sample and test fluid shall be at equilibrium, ‘with normal room temperature. 9. Procedure 9.1 Submerge the specimen in fluid contained in the vessel within the vacuum chamber. The uppermost surface of the specimen shall be covered by not less than 1 in. 25 mm) of uid, [Nort 11 or more stall packages maybe teste athe seme une, provided that they are placed sn sich & manner that all pats of avery package under tt can he observed for leakage during the Tes 9.2 Set the cover on the vacuum chamber, close the outlet valve, and turn on the vacuum so that the gauge rises slowly (approximately | in, Hy’) to a selected vacuum level. The ‘vacuum level chosen should he as large as possible in orker to ensure optimal sensitivity of the test. Limiting factors. will include package fragility, the degree of package expansion, and! the test-fluid vapor pressure 9.3 During the rise in vacuum, observe the submerged specimen for leakage in the form of a steady progression of bubbles from the flexible container. Isolated bubbles caused by enisapped ait are noe considered as leaks. Also note the approximate increase in package volume. The pressure differ- ential of the testis inversely related to the volume increase of the sample; therefore, large volume increases. significantly ddtract from the severity of the test, Flexible packaging with litle or no headspace cannot be reliably evalusted with this test method. 94 Hold the vacuum for a specificd time period 30 5 is recommended, but this may he Set at the tster's discretion, 9.5 Release the vacuum, remove the lid, and examine the specimen for the presence of test fluid inside the specimen. 10, Interpretation of Results, 10.1 there ate bubbles definitely attributable to Teaks in a specimen during the rise of vacuum, oc when held at full ‘vacuum, the specimen fails the tes. 10.2 If test fluid attributable to a leak is inside a specimen, the specimen fails the test, 10.3 If there are no bubbles observed attributable to leaks, sind if no test Muid attributable w 2 leak is inside a specimen, the specimen passes the tet, A. Report 11.1 Report the following information: ILA A statement that the test was conducted in compli- ‘ance with this test method or a description of the deviations from this test method 11.1.2. Kentification of the specimen and the specific mate rial tesied, 1112.1 Identification of the test fuid and the maximum vacuum level employed: 1.1.2.2 A statement regarding the approximate average and range of sample expansions when at maximum vacuum; and 11.1.2.3 The time period held at maximum vacuum. 11.13 A statement whether or aot leakage oceurred, and if possible, a report of the location of each leak. 11.1.4 A statement of the number of specimens included in the test and the number of failures, if any. 11.5 When the testis performed to check compliance with requirements, a statement that the sample did or did not meet the requirement, and identification of the source for the requirement. 11.1.6 When the test is conducted to evaluate or compare producis, materials, or methods, a statement of any observa tions that may lea to improvements Precision and Bias 12.1 An interlaboratory test was conducted to determine each participating laboraory’s ability to detect leaks of various sizes when tested al various vacuum levels in accordance with the test method, Ifa leak was detected, the participant was then asked to quantify the size of the leak by deiermining the time required 10 leak 4 mL. of air 12.1.1 Details ofthe test protocol, ineluding a description of the apparatus, are in preparation and will be available as a research report. 12.1.2 Three laboratories participated with each providing three independent researchers. Each of these tests were repli- ‘cated three times by each researcher. The same measured leaks ‘and test apparatus were used at each location 12.13 The three vacuum levels tested (“low”, “medium,” ‘and “high” were relative terms used only to differentiate conditions), were ow vaca 125405in Hy Merten eae vasa0sm Hp on vaca 2654051 Hp 12.14 The leaks used ¢big”, “medium,” “small.” and “very sinall” were relative terms used only 1o differentiate variables) wore characterized by a helium leak detector as listed below, By most siandards, all of these leaks were ite large Be 6602 cos he Mest TE ons He Sra E03 so He vary ra TE oes He unoring dts ve heen at AST Ineratonl Headyarer and my techusaed by repesting Mesa Roa RBI 1D, Contet ASTM Coserfy 03078 — 12.15 Precision, characterized by repeatability, Sir and reproducibility, $R, R has been determined for the materials us 02 (2021)** With this medium level of vacaum (18 in. Hg), the “very small” leak produced a bubble | time out of 27 trials. This is shown ia the tables that follow. essentially “non-detectable.” All ogher leaks. were easily de- 12.1.6 Values reported below are in seconds to leak YS mL tected, of ir except for the last material, “very small”, which Was 9.1.9 Precision Statement for Test Condition: High either reported as bubble produced within 1 min (1) or 90 bubble produced (0). ae ae 12.1.7 Precision Statement for Test Condition: Low Vacuum = ms £ - r * (2 in, He) sa tose) tm ate zee ae ‘Materials Average Sr oF . f ae vein Scorer 4050 4eee a1 By 04.778 re 1419020762 39721 a Se sal io0sr zh anne aren ence eos tee EIS eet eee et Voyemal 077 0000 oat) ceo 1.205 ‘Small 798.148 90264 = 100.144 84758 280.404 Tee we too nom bum com out With this highest vacuum level sed (24 in. Hi), the “very “ee sina” leak produced « bubble in 78% ofthe rials. This seems Under this relatively weak vacuum (12 in, Hg), the “very small” leak at | E-04 ce/s Helium did not precuce any bubbles within 1 min, which is taken as “aon-detectable.” All other leaks were easily detected, 12.L8 Precision Statement for Test Condition: Medium ‘Vacuum (18 in. He) to indicate that a leak of the size of | E-04 is “detectable” most ‘of the time but is elose to the detection limit of the method and test conditions 13, Keywords 13.1 bubble emission; determination: flexible packaging: Meiosis Average S} SR leaks aie ear aoe gate 74a? 10671 Medun ges Agra ot98 | HH408 t7080 703 ma xes00o 189m caste sce ot E03 Veyemal G07 ono2 0.2m ass wean ASTU nteratoral ahs re posite spacing te vay of ary pton ight aseredm cemacten wih any tem mentioned sn tcsaraard Usir fa stra ar expinay sere fa atominsbor of easy CF any sie pated i: apd Mek of nvegmant ol such igh, ara ately tau own asperstly "Tes sarc suect 6 rvs a ary tne by te responsible wecricetcormitee and ru be reviewed rere years nd ‘rnottense, ete reoprovedor alta. You caronens er edie fo evs offs lana a fy a0sone ards and should bo aktessed 0 ASTM rteratora eaauarers ou comments wil fecvecarky corsterao ae newly of he ‘expanse tsctvce corenitee, wish you mey etre Hyer fel tn four cernerts ave mo rctved Rear as dd ‘make you vows hrown tote ASTM Conontos et Serta, alt aes she baton The tard ecoyighd by ASTM Inbertional 100 Bar Harbor ive, PO Box C700, Viet Conerohockon, PA 10128-2959, Unted Stator. nau rapes (ingle or mute copes) ef ths standeri may ba abtaod by contacting ASTM at Ve above address o7 af B10-8%2.9535 (chore), BIOSSO-GSSS (fax, or sovice Basimoxy (o-nal) of tnrigh the ASTY wobsie {trawasimorg) Poomssen rons ta pretacany Mo standard may sleo 00 sceurea Yom the Copynght Clstanes Cont! 222 Foseweed Drv, Danvers, Mi 01823 Tel 878) SIS2600;hipvmiceryghcom