1、Designation: F3287 171Standard 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 y
2、ear 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.1NOTEEditorial corrections were made in May 2018.1. Scope1.1 This method provides a nondestructive means to detectholes (le
3、aks) in a variety of non-porous rigid and semi-rigidpackages.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 thetes
4、t cycle. The closed system includes a vacuum reservoir,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
5、 vacuum reservoir is measured by the IMFS.Based on 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 qualitative (pass/fail) results depending on the require-ments.1.2.1
6、 Headspace gas leakage defects equivalent to a 1mdiameter 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 leaka
7、ge defectsequivalent toa2mdiameter glass micropipette 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
8、with its use. It is theresponsibility of the user 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 recognize
9、d principles on standard-ization established in 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
10、the Terms Precision and Bias inASTM Test MethodsE691 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 labor
11、atories3. Terminology3.1 For terminology related to primary 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 p
12、ackage (material type,labels, etc.).3.2.2 blank master part, na piece of metal tooling withsimilar volume and shape as the actual test package. This isused to represent a leak free package.1This test method is under the jurisdiction ofASTM Committee F02 on PrimaryBarrier Packaging and is the direct
13、responsibility of Subcommittee F02.40 onPackage Integrity.Current edition approved Nov. 1, 2017. Published November 2017. DOI:10.1520/F3287-17.2Mass Extraction is covered by patents (1, 2). If you are aware of analternative(s) to the patented item, please attach to your ballot return a descriptionof
14、 the alternatives. All suggestions will be considered by the committee. Ifalternatives are identified, the committee 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.a
15、stm.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.4Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036, http:/www.ansi
16、.org.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of
17、International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.13.2.3 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 to se
18、al thechamber lid onto the base. The chamber base also contains anest 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 abo
19、ve the chamber base.3.2.5 container closure integrity 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 independe
20、ntly qualified bysupplier. Flow paths of this 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
21、 beforethe chamber is fully evacuated. This step 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
22、measuring mass flow,pressure (vacuum) and temperature (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 chambe
23、r is fully evacuated. This step isintended to 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
24、(moisture removal) requirements.Refer to Section 10 for 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 packag
25、e capable of passing aerosols (micro-organisms 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 ir
26、regular shaped with given throat area (smallestcross 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 rea
27、l life leaks. Theglass micropipette is encapsulated 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 tr
28、aceable standards in com-pliance with the requirements 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, IMF
29、S sensor, and controls tocomplete mass extraction 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 re
30、turn to original shape once vacuum isremoved.3.2.17 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 proce
31、ss that is equivalent orsuperior to distillation 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 i
32、llustrates the mass extraction test concept (3). 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. TheIMF
33、S measures mass flowing from the vacuum test chamberinto the vacuum reservoir. The mass flow is proportional to theFIG. 1 Micropipette Epoxied Inside Protective NeedleF3287 1712defect geometry at the given differential pressure. The mea-sured gas flow results from leaks from the headspace volume orl
34、iquid (e,g, water) leaks exposed to the vacuum inside thechamber. Since the vacuum pressure is lower than the boilingpoint 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 chambe
35、r design, package material type, andtest system 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 ma
36、ss into the vacuum test chamber due tooutgassing. 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 pack
37、aging or some label materials) test pack-age preparation 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 d
38、uring the test cycle will change thevolume inside 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 part
39、icularly significant for dry products where theinternal 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 l
40、eak test to detect the larger defects early in 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 adva
41、nce of fine leak measurement to ensure leaks of 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
42、 seal the package.Defects can allow unwanted gas (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
43、 products can be used toassure the stability of 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 areessent
44、ially unlimited, as long as a vacuum test chamber 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 p
45、rocess parameters.5.4 Applications for mass extraction 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 a
46、ble to detect defects if they become plugged bysolid 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 solut
47、ions. Product clogging propen-sity is a function 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
48、 recommended ifproduct-package units are to be 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 intendedprod
49、uct.6. Apparatus6.1 Mass Extraction Leak Detection 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
