1、Designation: F 2338 09Standard Test Method forNondestructive Detection of Leaks in Packages by VacuumDecay Method1This standard is issued under the fixed designation F 2338; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year
2、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 and semi-rigid
3、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 chamber containing t
4、he 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 evacuated to a pre
5、ssure 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 selected for the preci
6、sion 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 can be detected.
7、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 wires of 125 mi
8、n 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 TargetVacuum of 4E4 Pa
9、 (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 GasLeakage)Hole defects of at least 5 m in diameter can bedetected. Plastic bottles with screw caps were tested at a ta
10、rgetvacuum 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. The sensitivity of
11、both 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 target vacuum of
12、about +1 mbarabsolute.1.2.5 Flexible, Nonporous Packages (Gas or LiquidLeakage)Such packages may also be tested by the vacuumdecay method. Sensitivity data for flexible packages were notincluded in the precision and bias studies, although the use ofvacuum decay for testing such packages is well know
13、n.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 obtained with theintroduction
14、 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.1This test method is under the jurisdiction of ASTM Committee F02 on FlexibleBarrier Packaging and is the direct responsibi
15、lity of Subcommittee F02.40 onPackage Integrity.Current edition approved Jan. 1, 2009. Published February 2009. Originallyapproved in 2003. Last previous edition approved in 2007 as F 2338 07.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United
16、States.1.5 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 practices and determine the applica-bility of regulatory limitations prior to use.2. Refer
17、enced Documents2.1 ASTM Standards:2D 996 Terminology of Packaging and Distribution Environ-mentsE 691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test MethodF17 Terminology Relating to Flexible Barrier PackagingF 1327 Terminology Relating to Barrier Materials for
18、Medi-cal Packaging33. Terminology3.1 DefinitionsFor definitions used in this test method,see Terminologies D 996, F17, and F 1327.3.2 Definitions of Terms Specific to This Standard:3.2.1 baseline vacuum decay, nthe extent of vacuumchange within the test chamber over time demonstrated by acontrol, no
19、n-leaking package.3.2.2 control, non-leaking packages, npackages withoutdefects and properly sealed or closed according to manufac-turers specifications.3.2.3 flexible, nonporous packages, npackages that sig-nificantly deflect when under vacuum, and are constructed ofmalleable, nonporous materials.
20、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, nonporous packages, npackages that do notsignificantly deflect und
21、er 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, ntrays made of materialthat retain shape upon deflection.
22、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 distinctive pattern ofdots, spotting or mottling on the tray sealin
23、g surface after thelid is removed.3.2.9 volumetric airflow meter, na calibration tool thatcan be used to provide an artificial leak of known volumetricairflow rate into the test chamber for verification of instrumentsensitivity. Airflow meters should be calibrated to NISTstandards. The operational r
24、ange 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 establishing accept/reject limits,see Annex A1.2For referenced A
25、STM 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 onthe ASTM website.3Withdrawn. The last approved version of this historical standard is reference
26、don www.astm.org.TABLE 1 Summary of Vacuum Decay Leak Tests Applications for Various Product-Packages SystemsPackage ExamplesAPackage Content Examples ASTM P therefore testresults reflect operator, laboratory and instrument variability.Another single laboratory study was run testing the samevacuum d
27、ecay instruments ability to detect air flow leaksintroduced into in test chambers containing packages withvarious 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 sum
28、marized inTable 2, two populations of non-lidded trays representing twotray sizes were tested. Defective samples contained 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
29、, while the otherthree trays were consistently identified as leaking. At thecompletion of the study, the two suspect 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 clo
30、gged. These two trayswere eliminated from the precision statement.(2) Porous Barrier Lidded TraysThe test method is 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 aTarg
31、et Vacuum of 4E4 Pa (400 mbar). As per the resultsoutlined in Table 3, two populations of porous barrier liddedtray 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 thetra
32、y wall (50 m or 100 m in diameter), and packages with asingle seal channel defect created using a wire of either 75 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 bere
33、liably verified.(3) Porous Barrier Lidded Trays with Various AdhesiveBonding SystemsThe test method is able to reliably 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
34、(400 mbar). Table 4 documents test results using two popu-lations of tray packages with porous barrier lidding materialrepresenting two seal bonding adhesive systems. All liddingmaterials consisted of the same porous barrier substrate.Adhesives included dot matrix (C) and continuous (D) sys-tems. De
35、fective samples with incomplete seal bonding wereincluded. For dot matrix adhesive seals, defect severity wasvisually 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
36、used to classify packages.(4) Trays with Various Porous Barrier Lidding MaterialsThe test method can be used to test packages sealed withvarious porous barrier lidding material types, and tests aresimilar in sensitivity (approximately E-2 Pam3s-1 at a TargetVacuum of 4E4 Pa 400 mbar). Table 5 summar
37、izes asingle laboratory study run using a single pressure transducer(gauge) vacuum decay instrument4to verify the test methodsability to evaluate semi-rigid thermoformed tray packagessealed with various porous barrier lidding material types, andto obtain an estimate of the tests sensitivity.5Critica
38、l test4Model Pti VeriPac 225 by Packaging Technologies and Inspection, 145 MainStreet, Tuckahoe, NY 10707. See Note 11.5Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR: F021019.TABLE 2 Gas Leak Detection ResultsNonlidded TrayAppr
39、oximateTray Size (cm)L 3 W 3 HTray DescriptionNumber ofUnits TestedTotal Number ofReplicate TestsNumber FAILED(Leaks detected)Number PASSED(No leaks detected)Success Rate(% accuratereplicate tests)14 3 7 3 2 No defect 5 45 0 45 100100 m hole 4 36 36 0 10017 3 13 3 2 No defect 5 45 0 45 10050 m hole
40、5 45 35 10A78 (100)A100 m hole 5 45 45 0 100ATwo test packages yielded all 10 PASS observations. An independent test laboratory later verified that the holes in these packages could no longer be located andmay have become clogged. In this case, the success rate is reported considering all 5 test tra
41、ys (78 %), and considering only the 3 known defective trays (100 %).F2338097parameters were identified for each package population. Eachtests sensitivity was determined by introducing air via acalibrated volumetric airflow meter into the instrument testchamber containing the test package. The tests
42、sensitivity wasdefined as the leak rate that first triggered FAIL test results.12.1.1.2 Rigid, Nonporous PackagesTwo studies, oneevaluating rigid HDPE bottles with induction seals and screw-caps, and another evaluating glass syringes with stakedneedles, were performed utilizing two differently desig
43、nedinstruments to detect gas leaks in rigid, nonporous packages.These studies are described below.(1) HDPE BottlesThe test method 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
44、 of 5E4 Pa (500 mbar). Nocontrol packages were falsely rejected. Test method is able todetect a calibrated gas flow rate of 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 v
45、acuum decay instruments,designed with a pressure transducer (gauge) combined with adifferential pressure transducer,6to verify the test methodsability to evaluate rigid, nonporous packages, and to obtain anestimate of the tests sensitivity.7The packages tested includedtwo sizes of plastic (HDPE) bot
46、tles, 30-mL and 75-mLcapacity, sealed with induction seals, and capped with non-child-resistant screw-thread caps (for the 30-mL bottles) and6Model Pti VeriPac 325 by Packaging Technologies and Inspection, 145 MainStreet, Tuckahoe, NY 10707. See Note 11.7Supporting data have been filed at ASTM Inter
47、national Headquarters and maybe obtained by requesting Research Report RR: F021020.TABLE 3 Gas Leak Detection ResultsTrays with Porous Barrier LiddingApproximatePackage Size(L 3 W 3 H)Porous BarrierLidding MaterialPackage DescriptionNumber ofPackage UnitsTestedTotal Numberof ReplicateTestsNumber FAI
48、LED(Leaks detected)Number PASSED(No leaks detected)Success Rate(% accuratereplicate tests)196 cm3(14 3 7 3 2)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
49、 100536 cm3(16.5 3 13 3 2.5)A No defect 5 45 0 45 10050 m hole 5 45 16 29 36100 m hole 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(L 3 W 3 H)Porous BarrierLidding MaterialBondingAdhesiveAPackage DescriptionNumber ofPackage UnitsTestedTotal Numberof ReplicateTestsNumber FAILED(Leaks
