1、Designation: F2338 09 (Reapproved 2013)Standard Test Method forNondestructive Detection of Leaks in Packages by VacuumDecay Method1This standard is issued under the fixed designation F2338; the number immediately following the designation indicates the year oforiginal adoption or, in the case of rev
2、ision, the 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 Test PackagesPackages that can be nondestructivelyevaluated by this test method include:1.1.1 Rigid
3、 and semi-rigid non-lidded trays.1.1.2 Trays or cups sealed with porous barrier liddingmaterial.1.1.3 Rigid, nonporous packages.1.1.4 Flexible, nonporous packages.1.2 Leaks DetectedThis test method detects package leaksby measuring the rise in pressure (vacuum loss) in an enclosedevacuated test cham
4、ber containing the test package. Vacuumloss results from leakage of test package headspace gasesand/or volatilization of test package liquid contents located inor near the leak. When testing for leaks that may be partially orcompletely plugged with the packages liquid contents, the testchamber is ev
5、acuated to a pressure below the liquids vapor-ization pressure. All methods require a test chamber to containthe test package and a leak detection system designed with oneor more pressure transducers. Test method sensitivities citedbelow were determined using specific product-package sys-tems select
6、ed for the precision and bias studies summarized inTable 1. Table 1 also lists other examples of relevant product-package systems that can be tested for leakage by vacuumdecay.1.2.1 Trays or Cups (Non-lidded) (Air Leakage)Hole orcrack defects in the wall of the tray/cup of at least 50 m indiameter c
7、an be detected. Nonlidded trays were tested at aTarget Vacuum of 4E4 Pa (400 mbar).1.2.2 Trays Sealed with Porous Barrier Lidding Material(Headspace Gas Leakage)Hole or crack defects in the wallof the tray/cup of at least 100 m in diameter can be detected.Channel defects in the seal area (made using
8、 wires of 125 min diameter) can be detected. Severe seal bonding defects inboth continuous adhesive and dot matrix adhesive packagesystems can be detected. Slightly incomplete dot matrixadhesive bonding defects can also be detected. All porousbarrier lidding material packages were tested at a Target
9、Vacuum of 4E4 Pa (400 mbar). The sensitivity of the test forporous lidded packages is approximately E-2 Pam3s-1using acalibrated volumetric airflow meter.1.2.3 Rigid, Nonporous Packages (Headspace Gas Leak-age) Hole defects of at least 5 m in diameter can bedetected. Plastic bottles with screw caps
10、were tested at a targetvacuum of 5E4 Pa (500 mbar). Using a calibrated volumet-ric airflow meter, the sensitivity of the test is approximatelyE-3.4 Pam3s-1.Air-filled glass syringes were tested at a targetvacuum of 7.5E4 Pa (+250 mbar absolute) and again at atarget vacuum of about +1 mbar absolute.
11、The sensitivity ofboth tests is approximately E-4.1 Pam3s-1using a calibratedvolumetric airflow meter.1.2.4 Rigid, Nonporous Packages (Liquid Leakage)Holedefects of at least 5 m in diameter can be detected. Thisdetection limit was verified using a population of water-filledglass syringes tested at a
12、 target vacuum of about +1 mbarabsolute.1.2.5 Flexible, Nonporous Packages (Gas or Liquid Leak-age) Such packages may also be tested by the vacuum decaymethod. Sensitivity data for flexible packages were not in-cluded in the precision and bias studies, although the use ofvacuum decay for testing suc
13、h packages is well known.1.3 Test ResultsTest results are qualitative (Accept/Reject). Acceptance criteria are established by comparingquantitative baseline vacuum decay measurements obtainedfrom control, non-leaking packages to measurements obtainedusing leaking packages, and to measurements obtain
14、ed with theintroduction of simulated leaks using a calibrated gas flowmeter.1.4 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.5 This standard does not purport to address all of thesafety concerns, if any, associated with its
15、 use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.1This test method is under the jurisdiction of ASTM Committee F02 on FlexibleBarrier Packaging and is the direct re
16、sponsibility of Subcommittee F02.40 onPackage Integrity.Current edition approved Aug. 1, 2013. Published September 2013. Originallyapproved in 2003. Last previous edition approved in 2009 as F2338 09. DOI:10.1520/F2338-09R13.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Cons
17、hohocken, PA 19428-2959. United States12. Referenced Documents2.1 ASTM Standards:2D996 Terminology of Packaging and Distribution Environ-mentsE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test MethodF17 Terminology Relating to Flexible Barrier PackagingF1327 Te
18、rminology Relating to Barrier Materials for Medi-cal Packaging (Withdrawn 2007)33. Terminology3.1 DefinitionsFor definitions used in this test method, seeTerminologies D996, F17, and F1327.3.2 Definitions of Terms Specific to This Standard:3.2.1 baseline vacuum decay, nthe extent of vacuumchange wit
19、hin the test chamber over time demonstrated by acontrol, non-leaking package.3.2.2 control, non-leaking packages, n packages withoutdefects and properly sealed or closed according to manufac-turers specifications.3.2.3 flexible, nonporous packages, npackages that sig-nificantly deflect when under va
20、cuum, and are constructed ofmalleable, nonporous materials. Examples include pouches orbags made of polymeric, foil, or laminate films.3.2.4 gas leaks, nleak paths that allow the flow of gasfrom the test package.3.2.5 liquid leaks, nleak paths partially or fully filled withliquid.3.2.6 rigid, nonpor
21、ous packages, npackages that do notsignificantly deflect under vacuum and are constructed of solid,nonporous materials. Examples include plastic bottles withscrew-thread or snap-on closures, glass or plastic vials withelastomeric closures, and glass or plastic syringes.3.2.7 semi-rigid trays or cups
22、, ntrays made of materialthat retain shape upon deflection. For example, thermoformedPETE or PETG trays are considered semi-rigid trays.3.2.8 spotty or mottled seals, nan incomplete adhesivebond made between a package tray or cup and porous liddingmaterial that can be visibly identified by a distinc
23、tive pattern ofdots, spotting or mottling on the tray sealing surface after thelid is removed.3.2.9 volumetric airflow meter, na calibration tool that canbe used to provide an artificial leak of known volumetricairflow rate into the test chamber for verification of instrumentsensitivity. Airflow met
24、ers should be calibrated to NISTstandards. The operational range of the meter should reflect thedesired limit of sensitivity for the intended leak test.3.3 Definitions of Test Cycle and Critical ParametersTermsFor terms and abbreviations relating to the test cycleand the critical parameters for esta
25、blishing accept/reject limits,see Annex A1.4. Summary of Test Method4.1 The test package is placed in a test chamber to whichvacuum is applied. The chamber is then isolated from the2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.or
26、g. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3The last approved version of this historical standard is referenced onwww.astm.org.TABLE 1 Summary of Vacuum Decay Leak Tests Applications for Various Product-Packages SystemsPack
27、age ExamplesAPackage Content Examples ASTM P therefore testresults reflect operator, laboratory and instrument variability.Another single laboratory study was run testing the samevacuum decay instruments ability to detect air flow leaksintroduced into in test chambers containing packages withvarious
28、 porous barrier lidding material types.(1) Nonlidded TraysThe test method is able to identifydefective trays with holes 50 m, when using a TargetVacuum (Vac) of 4E4 Pa (400 mbar). As summarized inTable 2, two populations of non-lidded trays representing twotray sizes were tested. Defective samples c
29、ontained a singlehole in the tray wall of either 50 m or 100 m in diameter.Two of the five larger trays, each with a 50 m hole, repeatedlyfailed to be detected at more than one test site, while the otherthree trays were consistently identified as leaking. At thecompletion of the study, the two suspe
30、ct trays were indepen-dently reexamined for the presence and size of the holes. It wasdetermined that the holes could no longer be located and it washypothesized that they had become clogged. These two trayswere eliminated from the precision statement.(2) Porous Barrier Lidded TraysThe test method i
31、s ableto identify defective packages sealed with porous barrierlidding material, tray holes of at least 100 m in diameter, andchannel defects created using a 125 m wire, when using aTarget Vacuum of 4E4 Pa (400 mbar). As per the resultsoutlined in Table 3, two populations of porous barrier liddedtra
32、y packages were tested, representing two package sizes, allsealed with one type of coated porous barrier lidding material.Defective samples included packages with a single hole in thetray wall (50 m or 100 m in diameter), and packages with asingle seal channel defect created using a wire of either 7
33、5 m,100 m, or 125 m in diameter (0.003, 0.004, and 0.005 in.,respectively). An independent laboratory microscopically veri-fied tray hole sizes, however seal channel sizes could not bereliably verified.(3) Porous Barrier Lidded Trays with Various AdhesiveBonding Systems The test method is able to re
34、liably identifypackages with less than optimum seal bonding for dot matrixadhesive systems, and severely incomplete bonds made withcontinuous adhesive systems at a Target Vacuum of 4E4 Pa(400 mbar). Table 4 documents test results using two popu-lations of tray packages with porous barrier lidding ma
35、terialrepresenting two seal bonding adhesive systems. All liddingmaterials consisted of the same porous barrier substrate.Adhesives included dot matrix (C) and continuous (D) sys-tems. Defective samples with incomplete seal bonding wereincluded. For dot matrix adhesive seals, defect severity wasvisu
36、ally judged at the independent laboratory where the pack-ages were sealed. Continuous adhesive seals could not bevisually verified with accuracy; therefore, only sealing condi-tions were used to classify packages.(4) Trays with Various Porous Barrier Lidding MaterialsThe test method can be used to t
37、est packages sealed withvarious porous barrier lidding material types, and tests aresimilar in sensitivity (approximately E-2 Pam3s-1at a TargetVacuum of 4E4 Pa 400 mbar). Table 5 summarizes asingle laboratory study run using a single pressure transducer(gauge) vacuum decay instrument4to verify the
38、test methodsability to evaluate semi-rigid thermoformed tray packagessealed with various porous barrier lidding material types, andto obtain an estimate of the tests sensitivity.5Critical test4Model Pti VeriPac 225 by Packaging Technologies and Inspection, 145 MainStreet, Tuckahoe, NY 10707. See Not
39、e 11.5Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:F02-1019.TABLE 2 Gas Leak Detection ResultsNonlidded TrayApproximateTray Size (cm)LWHTray DescriptionNumber ofUnits TestedTotal Number ofReplicate TestsNumber FAILED(Leaks det
40、ected)Number PASSED(No leaks detected)Success Rate(% accuratereplicate tests)1472 Nodefect 5 45 0 45 100100 m hole 4 36 36 0 10017 13 2 No defect 5 45 0 45 10050 m hole 5 45 35 10A78 (100)A100 m hole 5 45 45 0 100ATwo test packages yielded all 10 PASS observations. An independent test laboratory lat
41、er verified that the holes in these packages could no longer be located and mayhave become clogged. In this case, the success rate is reported considering all 5 test trays (78 %), and considering only the 3 known defective trays (100%).F2338 09 (2013)7parameters were identified for each package popu
42、lation. Eachtests sensitivity was determined by introducing air via acalibrated volumetric airflow meter into the instrument testchamber containing the test package. The tests sensitivity wasdefined as the leak rate that first triggered FAIL test results.12.1.1.2 Rigid, Nonporous PackagesTwo studies
43、, oneevaluating rigid HDPE bottles with induction seals and screw-caps, and another evaluating glass syringes with stakedneedles, were performed utilizing two differently designedinstruments to detect gas leaks in rigid, nonporous packages.These studies are described below.(1) HDPE BottlesThe test m
44、ethod is able to identifydefective packages with holes at least 5 m in diameter, with ahigh probability of detecting hole sizes even smaller than 5 m,when using a Target Vacuum of 5E4 Pa (500 mbar). Nocontrol packages were falsely rejected. Test method is able todetect a calibrated gas flow rate of
45、between 0.25 and 0.27 ccm(equivalent to a volumetric flow rate at target vacuum of E3.4to E3.3 Pam3s-1). Table 6 summarizes a single laboratorystudy run using three identical vacuum decay instruments,designed with a pressure transducer (gauge) combined with adifferential pressure transducer,6to veri
46、fy the test methodsTABLE 3 Gas Leak Detection ResultsTrays with Porous Barrier LiddingApproximatePackage Size(LWH)Porous BarrierLidding MaterialPackage DescriptionNumber ofPackage UnitsTestedTotal Numberof ReplicateTestsNumber FAILED(Leaks detected)Number PASSED(No leaksdetected)Success Rate(% accur
47、atereplicate tests)196 cm3(1472)A No defect 5 45 2 43 9650 m hole 5 45 36 9 80100 m hole 5 45 45 0 100Channel made with 75 m wire 5 45 15 30 33Channel made with 100 m wire 5 45 45 0 100Channel made with 125 m wire 5 45 45 0 100536 cm3(16.5132.5)A No defect 5 45 0 45 10050 m hole 5 45 16 29 36100 m h
48、ole 5 45 45 0 100Channel made with 75 m wire 5 45 1 44 2Channel made with 100 m wire 5 45 40 5 89Channel made with 125 m wire 5 45 45 0 100TABLE 4 Gas Leak Test ResultsTrays with Porous Barrier Lidding Seal Bonding DefectApproximatePackage Size(LWH)Porous BarrierLidding MaterialBondingAdhesiveAPacka
49、ge DescriptionNumber ofPackage UnitsTestedTotal Numberof ReplicateTestsNumber FAILED(Leaks detected)Number PASSED(No leaksdetected)Success Rate(% accuratereplicate tests)536 cm3(16.5132.5)A C No defect 5 45 0 45 100Slightly incomplete bonding 5 45 45 0 100Severely incompletebonding5 45 45 0 100536 cm3(16.5132.5)A D No defect 5 45 0 45 100Slightly incomplete bonding 5 45 32 13 71Severely incompletebonding5 45 45 0 100ABonding adhesives were either continuou
