1、Designation: F3287 17Standard Test Method forNondestructive Detection of Leaks in Packages by MassExtraction Method1,2This standard is issued under the fixed designation F3287; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the ye
2、ar 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 method provides a nondestructive means to detectholes (leaks) in a variety of non-porous rigid and semi-rig
3、idpackages.1.2 This test method detects package leaks by measuring themass flow extracted from a package while the package isenclosed inside an evacuated test chamber. The test system isa closed system during the leakage measurement portion of thetest cycle. The closed system includes a vacuum reser
4、voir,Intelligent Molecular Flow Sensor (IMFS), and vacuum testchamber. Mass extracted from the test package into the vacuumtest chamber flows to the vacuum reservoir through the IMFSto equalize the system. Mass flow rate from the vacuumchamber to the vacuum reservoir is measured by the IMFS.Based on
5、 the conservation of mass law, mass flow into theclosed system is equal to the mass loss from the test package.The test system is capable of producing quantitative (variabledata) or quantitative (pass/fail) results depending on therequirements.1.2.1 Headspace gas leakage defects equivalent to a 1mdi
6、ameter glass micropipette (sharp edge defect) can be detectedat a 95% confidence level.1.2.2 Liquid leakage defects equivalent to a 1m diameterglass micropipette can be detected at a 95% confidence levelfor glass vials and LDPE bottles. Liquid leakage defectsequivalent to a 2m diameter glass micropi
7、pette can bedetected for glass syringes.1.3 UnitsThe values stated in SI units are to be regardedas standard. Pressure units are expressed as Pa, mbar, or Torr.1.4 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the use
8、r of this standard to establish appro-priate safety, health, and environmental practices and deter-mine the applicability of regulatory limitations prior to use.1.5 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in
9、the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:3E177 Practice for Use of the Terms Precision and Bias inASTM Test Methods
10、E691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test MethodF17 Terminology Relating to Primary Barrier Packaging2.2 ISO Standard:4ISO/IEC 17025 General requirements for the competence oftesting and calibration laboratories3. Terminology3.1 For terminology related
11、 to flexible barrier packaging,see Terminology F17.3.2 Definitions of Terms Specific to This Standard:3.2.1 baseline flow measurement, nmeasured flow rate fora negative control test package. Measured flow is largelyattributed to characteristics of the package (material type,labels, etc.).3.2.2 blank
12、 master part, na piece of metal tooling withsimilar volume and shape as the actual test package. This isused to represent a leak free package.3.2.3 chamber base, nlower portion of a vacuum testchamber that is connected to the mass extraction test instru-ment. Chamber base commonly includes an o-ring
13、 to seal thechamber lid onto the base. The chamber base also contains a1This test method is under the jurisdiction ofASTM Committee F02 on PrimaryBarrier Packaging and is the direct responsibility of Subcommittee F02.40 onPackage Integrity.Current edition approved Nov. 1, 2017. Published November 20
14、17. DOI:10.1520/F3287-17.2Mass Extraction is covered by a patents (1, 2). If you are aware of analternative(s) to the patented item, please attach to your ballot return a descriptionof the alternatives. All suggestions will be considered by the committee. Ifalternatives are identified, the committee
15、 shall reconsider whether the patented itemis necessary. The committee, in making its decision, shall follow Regulation 15.3For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, re
16、fer to the standards Document Summary page onthe ASTM website.4Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036, http:/www.ansi.org.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United Stat
17、esThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Tra
18、de (TBT) Committee.1nest to contain the test package. Nest configuration is depen-dent on test package features.3.2.4 chamber lid, nupper portion of a vacuum testchamber. The chamber lid commonly conforms to the portionof the test package that extends above the chamber base.3.2.5 container closure i
19、ntegrity test (CCIT), na methodto determine if a package is sealed to a specified level.3.2.6 glass micropipette, na thin glass tube that includes aspecific diameter within 620% of specification at the tip of thecapillary tube. Micropipettes are independently qualified bysupplier. Flow paths of this
20、 nature are commonly designated assharp edge (SE) holes. This can be used to represent a hole ofa specific diameter when inserted into a package.3.2.7 gross leak (GL) check, npreliminary step in the leakdetection process where chamber pressure is measured beforethe chamber is fully evacuated. This s
21、tep is intended to detectmajor issues (e.g. missing cap, chamber lid not installed,missing part, etc.).3.2.8 intelligent molecular flow sensor (IMFS), nmassflow measurement sensor that is capable of operating in thetransitional and molecular flow regimes measuring mass flow,pressure (vacuum) and tem
22、perature (3). The IMFS is indepen-dently calibrated against traceable standards per the require-ments of ISO 17025.3.2.9 large leak check (LLC), npreliminary step in theleak detection process where the mass exiting the chamber ismeasured before the chamber is fully evacuated. This step isintended to
23、 detect leaks large enough to allow the test packageto be evacuated as the vacuum test chamber is evacuated inpreparation for the fine leak test. This step is also intended todetect liquid leakage or spillage early in the process tominimize system drying (moisture removal) requirements.Refer to sect
24、ion 10for additional details regarding the dryingprocess. The size of defect that would be detected in this teststep is largely dependent on target fine leak detection level.3.2.10 leak, na hole, void, or defect in the wall or matedcomponents of a package capable of passing aerosols (micro-organisms
25、 or inert), liquid, or vapor from one side of the wallto the other. These can be passed under action of pressureand/or concentration differential across the wall and is inde-pendent of quantity of fluid flowing. Real life leaks are randomand typically irregular shaped with given throat area (smalles
26、tcross section area) and length.3.2.11 leak artifact, na test package that includes amanufactured defect. For this method, leak artifacts are pack-ages that include a glass micropipette to simulate a packageleak with a similar cross sectional area as real life leaks. Theglass micropipette is encapsu
27、lated inside a syringe needle andinserted into the needle so its tip is near the needle sharp pointas shown in Fig. 1. The metal needle provides mechanicalprotection to the fragile micropipette. Leak artifact flow rateswere verified using airflow NIST traceable standards in com-pliance with the requ
28、irements of ISO 17025 to assure theirintegrity and size.3.2.12 leak test signature, nflow curve that displays theflow rate for the test package through the test cycle.3.2.13 mass extraction instrument, ncomplete instrumentwith automated test circuit, IMFS sensor, and controls tocomplete mass extract
29、ion testing (3).3.2.14 negative control, nintact (known good) test pack-age.3.2.15 rigid packages, ntest packages that maintain theirshape with very minimal deflection under vacuum.3.2.16 semi-rigid packages, ntest packages that deformunder vacuum but return to original shape once vacuum isremoved.3
30、.2.17 verification orifice, ncalibrated leak device builtinto the mass extraction instrument includes a small calibratedleak used for periodic test system challenges.3.2.18 water for injection (WFI), nwater purified bydistillation or a purification process that is equivalent orsuperior to distillati
31、on in the removal of chemicals andmicroorganisms.4. Summary of Test Method4.1 The test package is placed inside a vacuum test chamberand the vacuum test chamber evacuated. The test systemincludes a vacuum reservoir, IMFS, and vacuum test chamber.Fig. 2 illustrates the mass extraction test concept (3
32、). Once thetest system is evacuated to the appropriate level, the system isisolated from the vacuum source. Mass extracted from the testpackage into the vacuum test chamber through any leakspresent in the package will flow to the vacuum reservoir. TheIMFS measures mass flowing from the vacuum test c
33、hamberinto the vacuum reservoir. The mass flow is proportional to thedefect geometry at the given differential pressure. The mea-sured gas flow results from leaks from the headspace volume orliquid (e,g, water) leaks exposed to the vacuum inside thechamber. Since the vacuum pressure is lower than th
34、e boilingFIG. 1 Micropipette Epoxied Inside Protective NeedleF3287 172point of water at 20 6 5 C, the liquid will boil resulting inliquid vapor and air gas flow mixture.4.2 Test system sensitivity is dependent on IMFS full scalerange, vacuum test chamber design, package material type, andtest system
35、 set-up parameters. Test system set-up parameterscan vary significantly based on required sensitivity, test pack-age material type, test package volume (size), and amount ofpackage deflection that occurs when vacuum is applied. Ma-terials can release mass into the vacuum test chamber due tooutgassin
36、g. The effects of outgassing on final mass flow ratecan be minimized by lengthening the evacuation time beforethe final mass flow rate is measured or raising the vacuum levelto a higher absolute pressure. In special cases (e.g. largevolume flexible packaging or some label materials) test pack-age pr
37、eparation may be required to minimize package volatiles.In cases where a component can move when vacuum is applied(e.g. Syringe or Cartridge stoppers), it is important to designthe vacuum test chamber to limit movement. Outward move-ment of components during the test cycle will change thevolume insi
38、de the vacuum test chamber and can cause flow tomove to the reservoir which could simulate a leaking packageor false positive.4.3 Test chamber and test parameters must be designed todetect large holes in packages (holes 70-100m in diameter).This is particularly significant for dry products where the
39、internal free volume inside the test package is evacuated. Largeleak detection for liquid filled packages is important tominimize introduction of liquid into the test system. Properchamber design and additional test steps are required prior tothe fine leak test to detect the larger defects early in
40、theevacuation process.NOTE 1A detailed description of the test steps, along with a sampletest signature, are included in AnnexA1.This additional information helpsto clarify the actions taken prior to fine leak measurements and precau-tions taken in advance of fine leak measurement to ensure leaks of
41、 all sizesare detected.5. Significance and Use5.1 Leaks in medical, pharmaceutical, or food productpackages can affect product quality and consumer safety. Suchleaks can arise from imperfections in package material orbetween mated components designed to seal the package.Defects can allow unwanted ga
42、s (e.g. oxygen or water vapor),particulates, liquids, or microbiological contaminants into orout of the package. Package defect detection can be a criticalpart of ensuring product quality and consumer safety. Use of aphysical CCI test method for sterile products can be used toassure the stability of
43、 the package sterility property duringtransportation and product shelf life.5.2 Mass extraction is a useful non-destructive test methodfor testing a wide variety of packages. Package shape anddimensions that can be tested using mass extraction areessentially unlimited, as long as a vacuum test chamb
44、er can bedesigned and manufactured to accommodate the package.5.3 This method produces quantitative flow measurementresults that are useful in comparing package sealing properties,different batches of product, material properties, and combina-tions of process parameters.5.4 Applications for mass ext
45、raction range from manuallyloaded and operated machines to automatic unattended workcells. This method can be applied for audit testing or 100%in-line testing.NOTE 2Leak test methods that rely on gas or vapor transport, such asmass extraction, are not able to detect defects if they become plugged by
46、solid or nonvolatile matter. Plugging is possible by exposure to environ-mental contaminants. In some cases, the packaged product itself can clogdefects. For example, leak paths may become blocked by suspendedsolids, gelatinous matter or dried-out solutions. Product clogging propen-sity is a functio
47、n of the product formulation, defect size and geometry, andmay be linked to product storage and handling conditions as well as thetime allotted to defect exposure. An investigation into the impact ofrepeated test condition exposure on defect plugging is recommended ifproduct-package units are to be
48、subject to repeated leak testing. Cloggingis a complex phenomenon that is not well characterized or understood.Care must be taken to ensure that any CCI test method based on gas orvapor transport through the leak path is appropriate for the intendedproduct.6. Apparatus6.1 Mass Extraction Leak Detect
49、ion ApparatusMass ex-traction apparatus includes a vacuum test chamber connectedto a test instrument that includes an IMFS. The system alsorequires a vacuum reservoir, vacuum generation package(pump, mixing tank, and regulator), and dry gas vent. Fig. 3includes a system photo and Fig. 4 includes a system overviewshowing the main components of a test system.6.2 Vacuum Test ChamberVacuum test chambers typicallyconsist of a chamber base and lid. The chamber base connectsto the mass extraction instrument and contains an o-ring to sealthe base to upper chambe
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