1、Designation: F2391 05 (Reapproved 2016)Standard Test Method forMeasuring Package and Seal Integrity Using Helium as theTracer Gas1This standard is issued under the fixed designation F2391; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revi
2、sion, 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 This test method includes several procedures that can beused for the measurement of overall package
3、and seal barrierperformance of a variety of package types and package forms,as well as seal/closure types. The basic elements of this methodinclude:1.1.1 Helium (employed as tracer gas),1.1.2 Helium leak detector (mass spectrometer), and1.1.3 Package/product-specific test fixtures.1.1.4 Most applica
4、tions of helium leak detection aredestructive, in that helium needs to be injected into the packageafter the package has been sealed. The injection site then needsto be sealed/patched externally, which often destroys itssaleability.Alternatively, if helium can be incorporated into theheadspace befor
5、e sealing, the method can be non-destructivebecause all that needs to be accomplished is to simply detectfor helium escaping the sealed package.1.2 Two procedures are described; however the supportingdata in Section 14 only reflects Procedure B (Vacuum Mode).The alternative, Sniffer Mode, has proven
6、 to be a valuableprocedure for many applications, but may have more variabil-ity due to exactly the manner that the operator conducts the testsuch as whether the package is squeezed, effect of multiplesmall leaks compared to fewer large leaks, background heliumconcentration, package permeability and
7、 speed at which thescan is conducted. Further testing to quantify this proceduresvariability is anticipated, but not included in this version.1.2.1 Procedure A: Sniffer Modethe package is scannedexternally for helium escaping into the atmosphere or fixture.1.2.2 Procedure B: Vacuum Modethe helium co
8、ntainingpackage is placed in a closed fixture. After drawing a vacuum,helium escaping into the closed fixture (capture volume) isdetected. Typically, the fixtures are custom made for thespecific package under test.1.3 The sensitivity of the method can range from thedetection of:1.3.1 Large leaks10-2
9、Pam3/s to 10-5Pam3/s (101cc/sec/atm to 10-4cc/sec/atm).1.3.2 Moderate leaks10-5Pam3/s to 10-7Pam3/s (10-4cc/sec/atm to 10-6cc/sec/atm).1.3.3 Fine leaks10-7Pam3/s to 10-9Pam3/s (10-6cc/sec/atm to 10-8cc/sec/atm).1.3.4 Ultra-Fine leak10-9Pam3/s to 10-11Pam3/s (10-8cc/sec/atm to 10-10cc/sec/atm).NOTE 1
10、Conversion from cc/sec/atm to Pam3/s is achieved bymultiplying by 0.1.1.4 The terms large, moderate, fine and ultra-fine are rela-tive terms only and do not imply the acceptability of any leakrate. The individual application dictates the level of integrityneeded. For many packaging applications, onl
11、y “large leaks”are considered unacceptable and the ability to detect smallerleaks is immaterial.All leak rates referred to in this method arebased on conversion of actual conditions (based on partialpressure of helium) to one atmosphere pressure differential andstandard temperature conditions.1.5 Th
12、e method may have applicability to any package type:1.5.1 Flexible,1.5.2 Semi-rigid, or1.5.3 Rigid.1.6 The sensitivities reported in the supporting data for thismethod pertain to the detectability of helium emanating fromthe sample and are not a function of the packaging form.1.7 The method is not a
13、pplicable to breathable or porouspackaging.1.8 The results obtained can be qualitative, semi-quantitative or quantitative depending on the procedure used.1.9 Test fixture design is not within the scope of this methodexcept to note that different designs will be needed for differentapplications (whic
14、h have different package types and packageintegrity requirements). Furthermore, the fixture selection anddesign will be based on where the testing is to be conductedwithin the manufacturing process (in other words, qualitycontrol versus research).1This test method is under the jurisdiction ofASTM Co
15、mmittee F02 on FlexibleBarrier Packaging and is the direct responsibility of Subcommittee F02.40 onPackage Integrity.Current edition approved April 1, 2016. Published April 2016. Originallyapproved in 2005. Last previous edition approved in 2011 as F2391 05(2011).DOI: 10.1520/F2391-05R16.Copyright A
16、STM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States11.10 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
17、health practices 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 EmissionD4991 Test Method for Le
18、akage Testing of Empty RigidContainers by Vacuum MethodE432 Guide for Selection of a Leak Testing MethodE479 Guide for Preparation of a Leak Testing Specification(Withdrawn 2014)3E493 Test Methods for Leaks Using the Mass SpectrometerLeak Detector in the Inside-Out Testing ModeE498 Test Methods for
19、Leaks Using the Mass SpectrometerLeak Detector or Residual Gas Analyzer in the TracerProbe ModeE499 Test Methods for Leaks Using the Mass SpectrometerLeak Detector in the Detector Probe ModeE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test MethodE1603 Test Met
20、hods for Leakage Measurement Using theMass Spectrometer Leak Detector or Residual Gas Ana-lyzer in the Hood ModeF17 Terminology Relating to Flexible Barrier PackagingF1327 Terminology Relating to Barrier Materials for Medi-cal Packaging (Withdrawn 2007)32.2 Other Documents:Principal author L. Kirsch
21、, et al - (shown in referenceAppendix X1 as literature references 1, 2, 3 and 5)Principal author L. Nguyen, et al - (shown in referenceappendix I at literature reference 4)Co-authors include C. Moeckly, L. Nguyen, R. Gerth, W.Muangsiri, R. Scheire, D. M. Guazzo, L. Kirsch, G.Schmitt,A. Kirsch, M. Ko
22、ch,T.Wertli, M. Lehman and G.Schramm.3. Terminology3.1 General Term DefinitionsFor definitions used in thisstandard see Terminology D996, Terminology F17 and Termi-nology F1327.3.2 Specific Term Definitions:3.2.1 actual helium leak rate (AHLR)Measured heliumleak rate (MHLR) signal level adjusted to
23、a driving force of100 % concentration at 101 KPa (1.0 atmosphere), absolute.3.2.2 breathable/porous packagingPackages, in whole orin part, that intentionally allow gases/vapors to flow freely intoand out of the package. (See also Terminology F1327)3.2.3 fine leaksFor the purpose of this test method,
24、 leaksthat exhibit gas/vapor leak rates between 110-7Pam3/s to10-9Pam3/s (110-6cc/sec/atmosphere to 110-8cc/sec/atmosphere).3.2.4 flexible packagingPackages (typically, pouches,sachets, and bags) constructed of materials that are readilybendable. (See also Terminology Method F17)3.2.5 impermeable pa
25、ckagingPackages constructed ofmaterials (typically metal or glass) that prevent gases/vaporsfrom flowing into or out of the package.3.2.6 large leaksFor the purpose of this test method, leaksthat exhibit gas/vapor leak rates between 110-2Pam3/s to110-5Pam3/s (1101cc/sec/atm to 110-4cc/sec/atmosphere
26、).3.2.7 measured helium leak rate (MHLR)Helium signallevel obtained based on the actual helium concentration in thepackage.3.2.8 moderate leaksFor the purpose of this test method,leaks that exhibit gas/vapor leak rates between 110-5Pam3/sto 10-7Pam3/s (110-4cc/sec/atmosphere to 110-6cc/sec/atmospher
27、e).3.2.9 outgassingThe release of adsorbed, absorbed orphysically trapped gas from a surface of structure.3.2.10 pass/fail criterionThe predetermined AHLR abovewhich the package being tested is considered defective and,therefore, unacceptable.3.2.11 permeable packagingPackages, in whole or in part,t
28、hat allow gases/vapors to flow into and out of a package viadiffusion controlled process.3.2.12 semi-rigid packagingPackages (typically, thermo-formable, or cold-formable materials) that are formed intoblisters or trays, with associated lidding materials applied asthe closure means.3.2.13 ultra fine
29、 leaksFor the purpose of this test method,leaks that exhibit gas/vapor leak rates between 110-9Pam3/sto 110-11Pam3/s (110-8cc/sec/atmosphere to 110-10cc/sec/atmosphere).3.2.14 virtual leakA source of detectable tracer gas otherthan from a defect of the seal or package. Such a virtual leakmay be the
30、result of membrane permeability, surface desorp-tion or release of trapped gas.4. Summary of Test Procedures4.1 There are two basic test procedures contained in this testmethod:4.1.1 Procedure ASniffer Mode.4.1.2 Procedure BVacuum Mode.4.2 Both of these test procedures require the package undertest
31、to have helium at some measurable level on the side of thepackage opposite the leak detector sensor (typically, the insideof the package). If the package cannot, or should not be sealedwith helium inside, the test fixture used for that particular test2For referenced ASTM standards, visit the ASTM we
32、bsite, 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.3The last approved version of this historical standard is referenced onwww.astm.org.F2391 05 (2016)2needs to p
33、rovide a means of helium introduction at theappropriate location and the appropriate time in the test cycle.The one exception is a package with a gross leak for which avariation of the helium pressurized “back-filling” or “soaking”technique may be applicable. In all cases helium, at as high aconcent
34、ration as practicable, must be present on one side of thepackage/seal barrier element.4.3 To quantify the leak rate level of a given package, orpackage seal, the partial pressure driving force of the heliummust be known. Therefore, an important part of the process ofconducting a leak rate test is th
35、e determination of the concen-tration of helium at one atmosphere (absolute pressure) presentduring the test. Generally speaking, some type of calibratedresidual gas analyzer (RGA) device will need to be utilized forthis step.4.4 The MHLR (measured helium leak rate) values will bedetermined based on
36、 a comparison to the calibration, referencestandard employed. It is subsequently adjusted to an AHLR(actual helium leak rate), which is based on the actual packagehelium partial pressure (see 4.5).4.5 If appropriate, the AHLR value for the package undertest can be compared to the pre-established Pas
37、s/Fail criterionfor that specific product/package to ascertain acceptability (perestablished specification requirements).5. Significance and Use5.1 The vacuum, bubble test method, as described in TestMethod D3078, and various other leak detection methodsdescribed elsewhere (Test Method D4991, Guide
38、E432, GuideE479, Test Method E493, Test Method E498, Test MethodE499, and Test Method E1603) have been successfully usedwidely in various industries and applications to determine thata given package is or is not a “leaker.” The sensitivity of anyselected leak test method has to be considered to dete
39、rmine itsapplicability to a specific situation.5.2 The procedures presented in this test method allow theuser to carry out package and seal integrity testing withsufficient sensitivity to quantify seals in the previously definedmoderate to very fine seal ranges.5.3 By employing seal-isolating leak t
40、esting fixtures, pack-ages constructed of various materials can be tested in the fullrange of seal performance requirements. Design of thesefixtures is beyond the scope of this method.5.4 These seal/package integrity test procedures can beutilized as:5.4.1 A design tool,5.4.2 For tooling qualificati
41、on,5.4.3 Process setup,5.4.4 Process validation tool,5.4.5 Quality assurance monitoring, or5.4.6 Research and development.6. Interferences6.1 The introduction of the helium tracer gas to the non-sensor side of the package (typically the inside) can be doneeither before or after sealing.6.2 Some heli
42、um may be present in the testing environmentwhich may interfere with results. Care must be taken toeliminate background helium with ventilation, location ofsupply cylinders, proper sample isolation fixturing or othermeans.6.3 When attempting to detect very small leaks, care mustbe taken to eliminate
43、, minimize, or compensate for falsereadings from “virtual leak” sources, particularly trappedhelium in seal areas.6.4 The permeation of the package by helium does notindicate a leak. Care must be taken to understand the level ofpermeation to prevent misinterpretation of results. Similarly,some mater
44、ials may absorb helium and yield false results whentested. Outgassing of these materials may greatly increase testtime.6.5 These procedures, particularly when detecting moderateto very fine leaks, should be carried out using calibratedexternal leak standards.6.6 Physical/mechanical constraints are g
45、enerally requiredfor flexible and semi-rigid packages to avoid vacuum-inducedseal failures. Properly constrained packages can mean thedifference between success and failure in carrying out the testprocedure.7. Apparatus7.1 A helium leak detector (mass spectrometer). An oil-freevacuum system is recom
46、mended with hard vacuum test portand sniffer probe attachment (as appropriate for a specificapplication) for those applications where the testing area needsto be maintained as a clean environment, or where the releaseof vacuum pump oil could lead to product contamination, orboth.7.2 External calibra
47、ted leaks (calibrated within the last 12months; 6 months is recommended). At least three rangesshould be covered depending on the application; typically110-6, 110-7and 110-8cc/s/atm. Alternatively, more cali-brated leaks may be used.7.3 Avacuum chamber, with custom-design constraints thatare package
48、-specific (sniffer mode testing may not require avacuum chamber).7.4 A headspace analyzer device for measuring the partialpressure of (concentration at 1 atm pressure) helium insamples.7.5 The method to introduce helium into the package needsto be developed specifically for the package under test.Te
49、chniques and devices that have been successfully employedinclude:7.5.1 Pre-filling of packages using an on-line floodingfixture (helium introduced to package headspace prior tosealing).7.5.2 Post-filling of packages by injection of helium into thesealed package.Afine gage syringe needle and flow-controlledhelium gas supply, followed by sealing of the puncture site hasbeen found to work well.F2391 05 (2016)37.6 An enclosure for sniffer mode testing seals/packages formoderate, fine, or ultra-fine leaks in a lowered helium
