1、Designation: F2228 02 (Reapproved 2007)F2228 13Standard Test Method forNon-Destructive Detection of Leaks in Medical PackagingWhich Incorporates Porous Barrier Material by CO2 TracerGas Method1This standard is issued under the fixed designation F2228; the number immediately following the designation
2、 indicates the year oforiginal adoption or, in the case of revision, 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 non-destructive test method dete
3、cts leaks in non-porous rigid thermoformed trays, as well as the seal between theporous lid and the tray. The test method detects channel leaks in packages as small as 100 m (0.004 in.) diameter in the seal aswell as 50 m (0.002 in.) diameter pinholes, or equivalently sized cracks in the tray, subje
4、ct to trace gas concentration in thepackage, package design and manufacturing tolerances.NOTE 1This test method does not claim to challenge the porous (breathable) lidding material. Any defects that may exist in the porous portion ofthe package will not be detected by this test method.1.2 The values
5、 stated in SI units are to be regarded as standard units. Values in parentheses are for information only.1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and
6、 health practices and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D996 Terminology of Packaging and Distribution EnvironmentsF17 Terminology Relating to Flexible Barrier PackagingF1327 Terminology Relating to Barrier Materials for Medi
7、cal Packaging (Withdrawn 2007)33. Terminology3.1 General Term DefinitionsFor definitions used in this standard, see Terminologies D996, F17, and F1327.3.2 Definitions of Terms Specific to This Standard:3.2.1 basal flowtransverse transport of trace gas across the seal due to gas flow within the plane
8、 of the porous barrier materialas well as flow between the porous barrier and the temporary gasketing. This is an expected property of the porous barrier materialand does not represent a leak. Experimentally, this flow may be thought of as noise, which will always be present, to some degree,during t
9、esting and must be accounted for.3.2.2 trace gasa compound selected solely for use to identify leakage flow.4. Summary of Test Method4.1 This test method utilizes CO2 sensing techniques in the detection of a CO2 trace gas to quantify leaks in medical packaging,which incorporates porous barrier mater
10、ial. This test method provides a qualitative (accept/reject) inspection method to evaluatepackages for pinhole, crack and channel leaks. Further information on the “Leak Test Theory” may be found in Annex A1.1 This test method is under the jurisdiction of ASTM Committee F02 on Flexible Barrier Packa
11、ging and is the direct responsibility of Subcommittee F02.40 on PackageIntegrity.Current edition approved April 1, 2007Aug. 1, 2013. Published May 2007September 2013. Originally approved in 2002. Last previous edition approved in 20022007 asF2228 02.F2228 02(2007). DOI: 10.1520/F2228-02R07.10.1520/F
12、2228-13.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.3 The last approved version of this historical standa
13、rd is referenced on www.astm.org.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recomm
14、ends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States15. Significance
15、 and Use5.1 Harmful biological or particulate contaminants may enter the package through incomplete seals or imperfections such aspinholes or cracks in the trays.5.2 After initial instrument set-up and calibration, the operations of individual tests and test results do not need operatorinterpretatio
16、n. The non-destructive nature of the test may be important when testing high value added products.5.3 Leak test results that exceed the permissible threshold setting are indicated by audible or visual signal responses, or both,or by other means.5.4 This non-destructive test method may be performed i
17、n either laboratory or production environments. This testing may beundertaken on either a 100 % or a statistical sampling basis. This test method, in single instrument use and current implementation,may not be fast enough to work on a production packaging line, but is well suited for statistical tes
18、ting as well as packagedevelopmental design work.6. Apparatus6.1 Non-destructive Trace Gas Leak Detection Apparatus ApparatusThe apparatus test fixture consists of three majorelements and is shown in Fig. 1.6.2 Sealing MembraneThe purpose of the sealing membrane is to seal off the tracer gas transmi
19、ssion, normal to the porouslid surface. However, the membrane does not completely control the transmission of tracer gas basal flow in the transversedirection.6.3 Control PackagesPackages with calibrated capillary channel leaks as well as packages with calibrated pinholes in the trayconstructed for
20、instrument calibration as well as for test procedure verification.6.4 Test FixtureApparatus, which must be designed to ensure detection of a calibrated leak.7. Preparation of Apparatus7.1 The test apparatus is to be started, warmed-up, and made ready according to the manufacturers specifications. Th
21、einstrument must be operated in an environment as described in the instruments user manual.8. Reagents and Materials8.1 CO2 Trace Gas Cylinder and Regulator A cylinder of “Commercial” or “Bone Dry” grade carbon dioxide with aminimum of 206.84 kPa (30 psi) pressure is required for calibration and tes
22、ting.FIG. 1 Schematic of Test Fixture and Test PackageF2228 1328.2 Sealing MembraneThe temporary sealing membrane must exhibit the correct pliability and tackiness in order to form agas-tight bond with the porous lidding materials during the testing process, and must release at the end of the test w
23、ithout damagingthe porous lid or the edge seal.8.3 Sealing Membrane-induced Damage During the process of membrane selection for a specific package design andconfiguration, inspect the packages for the following indications of membrane-induced damage after the membrane is removedfrom the package:8.3.
24、1 Sticky residue remaining on the porous barrier material at the end of the test cycle.8.3.2 Fibers from the porous barrier material remaining on the sealing membrane at the end of the test cycle.8.3.3 Visible changes to the texture or structure of the porous lidding material at the end of the test
25、cycle, under microscopeor other magnified examination.8.3.4 Damage to the printed information on the porous barrier. The adhesive of the sealing membrane may lift off the ink fromthe barrier.8.3.5 Failure of the package to release from the sealing membrane at the end of the test cycle.8.3.6 Damage t
26、o the seal incurred on removal of the membrane from the package.9. Hazards9.1 As the test fixture is closed, it may present pinch-point hazards.9.2 CO2, although inert and non-toxic, can cause danger of suffocation if it is allowed to displace oxygen. Thus it isrecommended that the spent carbon diox
27、ide be naturally vented away from the test area and that adequate ventilation be provided.10. Calibration and Standardization10.1 Before any measurements are made, the apparatus must be calibrated. The calibration procedure is used for overall systemcheckout, as well as to establish an initial refer
28、ence profile for a simulated channel or pinhole leak, and to determine test limitsfor each different package geometry that is to be tested using a specific test fixture. The calibration procedure is performed toestablish the sensitivity setting of the instrumentation. It is expected that the calibra
29、tion procedures are carried out frequently;typically, at least one or more times a day, preferably at the beginning of every shift.10.2 Refer to the instrument manufacturers operating instructions regarding preparation of Calibration Standards, Conditioningof Calibration Packages and Instrument Cali
30、bration used in establishing baseline settings.11. Procedure11.1 Verify that sufficient CO2 trace gas is available for the tests. Check the trace gas supply and functionality of the gas deliverysystem.11.2 Select and implement the properly sized test fixture for the packages to be tested. Verify tha
31、t the instrument and associatedtest fixture have been calibrated for the packages to be tested. The test fixture is too large when the instrument is unable to detecta calibrated control channel or pinhole leak.11.3 Adjust the instrument baseline settings determined in calibration.11.4 Place the pack
32、age assembly into the test fixture. Make certain that the package assembly is centered in the fixture and thatthe lidding side of the package is pointed up toward the test fixture hinged cover and incorporated sealing membrane.NOTE 2The sealing membrane needs to be clean in order to develop a good s
33、eal with the porous lidding of the package. Laboratory conditions maycause dust or debris to be collected on the sealing membrane. These conditions thus warrant frequent inspection and cleaning of the sealing membranewith a lint-free cloth soaked with a solvent recommended by the manufacturer of the
34、 equipment.11.5 Close the top cover of the test fixture and make certain that the CO2 port makes good contact with the package assembly.11.6 Start the test.11.7 Note the pass or fail indicator and record results. Set aside any “failed/defective” package for further evaluation. Furtherevaluation shou
35、ld include re-testing of the package.11.8 Select another package and repeat the testing process.12. Report12.1 The report shall include the following:12.1.1 A statement indicating that the tests were performed in accordance with ASTM Standard F2228, except where noted.12.1.2 The serial numbers, cali
36、bration values and most recent calibration dates for all calibration standards used.12.1.3 Record the date, time, location, and identification of the apparatus and the operator.12.1.4 Record the package type, size, material, product, and traceable identification numbers.12.1.5 Record the leak rate r
37、eject set point as programmed into the apparatus.12.1.6 Record the number of packages tested, and the number of failed packages.F2228 13312.1.7 Record the failed packages to be rejected by identifying either individual serial numbers or lot numbers.12.1.8 Record the disposition of good packages as w
38、ell as failed packages.12.1.9 Copies of any software-generated data sheets, or reports produced during the testing.13. Precision and Bias13.1 PrecisionA round robin study was conducted in 2002, which included three laboratories. Packages with and withoutchannels in the seal area and pinholes in the
39、trays were tested for leaks. The equipment used in this interlaboratory study was thePac Guard Model 500 available from MOCON.13.1.1 Two different package sizes were tested. The larger package consisting of a PETE tray and an adhesive coated 1073BTyvek lidding had the approximate outside dimensions
40、of 129 mm wide by 167 mm long by 20 mm high (5.1 by 6.6 by 0.8 in.)with an internal volume of 208 mL. The smaller package consisted also of a PETE tray and an adhesive coated 1073B Tyveklidding and had the approximate outside dimensions of 69 mm wide by 139 mm long by 18 mm high (2.7 by 5.5 by 0.7 i
41、n.) withan internal volume of 80.7 mL.13.1.2 Three sample packages for each of two sizes (six packages) contained a 100 m (0.004 in.) calibrated channel (leak),while six similar packages contained a 50 m (0.002 in.) calibrated pinhole (leak), and six similar packages contained a pluggedpinhole (no l
42、eak).13.1.3 Each sample material was tested at three laboratories, using the same instrumentation. Each package was tested at thetwo possible orientations allowed by the instrument. Two other operators subsequently repeated the tests at different times.Agrandtotal of 324 tests were performed, 216 on
43、 materials with leaks and 108 on materials without leaks.13.2 Tables 1-3 represent a summary of the test data.13.2.1 The results show that none of the 216 tests on calibrated leaks failed to detect the leak, that is, there were zero falsenegatives. Four of the 108 tests on plugged pinholes resulted
44、in the determination of a leak, that is, a false positive.13.2.2 Four errors occurred at Laboratory 2. It was observed that dust collected on the sealing membrane and thus proper sealingof the porous lidding may not have been accomplished. This condition would allow CO2 to flow between the sealing m
45、embraneand the package lidding into the test fixture where it would be detected and cause the alarm to be triggered. See Note 2 forinspection and cleaning guidelines for the sealing membrane.13.2.3 Aside from laboratory conditions, it can be argued that the instrument tests were independent, and tha
46、t the number ofdefects follows a binomial distribution with probability p of testing error. An estimate of p is the error rate, and a conservativeconfidence interval for p can be determined. The tables list the upper bound of a 95 % confidence interval for the true error rate.13.2.4 Package size had
47、 no effect on the test results.14. Keywords14.1 basal flow; carbon dioxide (CO2) leak testing; flexible packaging; infrared CO2 sensor; medical packaging; non-destructivetesting; package integrity monitoring; package integrity test; pass/fail criteria; pass/fail levels; permeable packaging; pinhole
48、leaks;porous barrier; porous lids; porous packaging; rigid thermoformed trays; sealing membrane performance; seal integrity monitoring;seal integrity test; seal leaks; sterile integrity tests; trace gas leak testingTABLE 1 Percent Incorrect by MaterialMaterial TestDeterminations IncorrectAnalysis Pe
49、rcent (%)Incorrect 95 % UpperBoundPackage 324 4 1.2 3.1F2228 134ANNEX(Mandatory Information)A1. LEAK TEST THEORYA1.1 Placing the lidded package in a test fixture to which the infrared sensor is connected initiates the test method. This methoddoes not locate the leak, but instead provides a measurement of total leakage. The response of the instrument to any leakage is anon-linear function of the leak (hole) size. The sensitivity of this method is a function of trace gas concentration in the package.It is recommended that the trace gas delivery flow be ad
