1、Designation: F 2228 02 (Reapproved 2007)Standard Test Method forNon-Destructive Detection of Leaks in Medical PackagingWhich Incorporates Porous Barrier Material by CO2TracerGas Method1This standard is issued under the fixed designation F 2228; the number immediately following the designation indica
2、tes 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 (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This non-destructive test method detects le
3、aks in non-porous rigid thermoformed trays, as well as the seal betweenthe porous lid and the tray. The test method detects channelleaks in packages as small as 100 m (0.004 in.) diameter in theseal as well as 50 m (0.002 in.) diameter pinholes, orequivalently sized cracks in the tray, subject to tr
4、ace gasconcentration in the package, package design and manufactur-ing tolerances.NOTE 1This test method does not claim to challenge the porous(breathable) lidding material. Any defects that may exist in the porousportion of the package will not be detected by this test method.1.2 The values stated
5、in SI units are to be regarded asstandard units. Values in parentheses are for information only.1.3 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 p
6、ractices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 996 Terminology of Packaging and Distribution Environ-mentsF17 Terminology Relating to Flexible Barrier PackagingF 1327 Terminology Relating to Barrier Materials for Medi-cal
7、 Packaging3. Terminology3.1 General Term DefinitionsFor definitions used in thisstandard, see Terminologies D 996, F 17, and F 1327.3.2 Definitions of Terms Specific to This Standard:3.2.1 basal flowtransverse transport of trace gas acrossthe seal due to gas flow within the plane of the porous barri
8、ermaterial as well as flow between the porous barrier and thetemporary gasketing. This is an expected property of theporous barrier material and does not represent a leak. Experi-mentally, this flow may be thought of as noise, which willalways be present, to some degree, during testing and must beac
9、counted for.3.2.2 trace gasa compound selected solely for use toidentify leakage flow.4. Summary of Test Method4.1 This test method utilizes CO2sensing techniques in thedetection of a CO2trace gas to quantify leaks in medicalpackaging, which incorporates porous barrier material. Thistest method prov
10、ides a qualitative (accept/reject) inspectionmethod to evaluate packages for pinhole, crack and channelleaks. Further information on the “Leak Test Theory” may befound in Annex A1.5. Significance and Use5.1 Harmful biological or particulate contaminants mayenter the package through incomplete seals
11、or imperfectionssuch as pinholes or cracks in the trays.5.2 After initial instrument set-up and calibration, the op-erations of individual tests and test results do not need operatorinterpretation. The non-destructive nature of the test may beimportant when testing high value added products.5.3 Leak
12、 test results that exceed the permissible thresholdsetting are indicated by audible or visual signal responses, orboth, or by other means.5.4 This non-destructive test method may be performed ineither laboratory or production environments. This testing maybe undertaken on either a 100 % or a statist
13、ical sampling basis.This test method, in single instrument use and current imple-mentation, may not be fast enough to work on a productionpackaging line, but is well suited for statistical testing as wellas package developmental design work.1This test method is under the jurisdiction of ASTM Committ
14、ee F02 on FlexibleBarrier Packaging and is the direct responsibility of Subcommittee F02.40 onPackage Integrity.Current edition approved April 1, 2007. Published May 2007. Originallyapproved in 2002. Last previous edition approved in 2002 as F 2228 02.2For referenced ASTM standards, visit the ASTM w
15、ebsite, 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.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United S
16、tates.6. Apparatus6.1 Non-destructive Trace Gas Leak Detection ApparatusThe apparatus test fixture consists of three major elements andis shown in Fig. 1.6.2 Sealing MembraneThe purpose of the sealing mem-brane is to seal off the tracer gas transmission, normal to theporous lid surface. However, the
17、 membrane does not com-pletely control the transmission of tracer gas basal flow in thetransverse direction.6.3 Control PackagesPackages with calibrated capillarychannel leaks as well as packages with calibrated pinholes inthe tray constructed for instrument calibration as well as fortest procedure
18、verification.6.4 Test FixtureApparatus, which must be designed toensure detection of a calibrated leak.7. Preparation of Apparatus7.1 The test apparatus is to be started, warmed-up, and madeready according to the manufacturers specifications. Theinstrument must be operated in an environment as descr
19、ibed inthe instruments user manual.8. Reagents and Materials8.1 CO2Trace Gas Cylinder and RegulatorA cylinder of“Commercial” or “Bone Dry” grade carbon dioxide with aminimum of 206.84 kPa (30 psi) pressure is required forcalibration and testing.8.2 Sealing MembraneThe temporary sealing membranemust
20、exhibit the correct pliability and tackiness in order toform a gas-tight bond with the porous lidding materials duringthe testing process, and must release at the end of the testwithout damaging the porous lid or the edge seal.8.3 Sealing Membrane-induced DamageDuring the pro-cess of membrane select
21、ion for a specific package design andconfiguration, inspect the packages for the following indica-tions of membrane-induced damage after the membrane isremoved from the package:8.3.1 Sticky residue remaining on the porous barrier mate-rial at the end of the test cycle.8.3.2 Fibers from the porous ba
22、rrier material remaining onthe sealing membrane at the end of the test cycle.8.3.3 Visible changes to the texture or structure of theporous lidding material at the end of the test cycle, undermicroscope or other magnified examination.8.3.4 Damage to the printed information on the porousbarrier. The
23、adhesive of the sealing membrane may lift off theink from the barrier.8.3.5 Failure of the package to release from the sealingmembrane at the end of the test cycle.8.3.6 Damage to the seal incurred on removal of themembrane from the package.9. Hazards9.1 As the test fixture is closed, it may present
24、 pinch-pointhazards.9.2 CO2, although inert and non-toxic, can cause danger ofsuffocation if it is allowed to displace oxygen. Thus it isrecommended that the spent carbon dioxide be naturally ventedaway from the test area and that adequate ventilation beprovided.10. Calibration and Standardization10
25、.1 Before any measurements are made, the apparatusmust be calibrated. The calibration procedure is used forFIG. 1 Schematic of Test Fixture and Test PackageF 2228 02 (2007)2overall system checkout, as well as to establish an initialreference profile for a simulated channel or pinhole leak, and todet
26、ermine test limits for each different package geometry thatis to be tested using a specific test fixture. The calibrationprocedure is performed to establish the sensitivity setting of theinstrumentation. It is expected that the calibration proceduresare carried out frequently; typically, at least on
27、e or more timesa day, preferably at the beginning of every shift.10.2 Refer to the instrument manufacturers operating in-structions regarding preparation of Calibration Standards, Con-ditioning of Calibration Packages and Instrument Calibrationused in establishing baseline settings.11. Procedure11.1
28、 Verify that sufficient CO2trace gas is available for thetests. Check the trace gas supply and functionality of the gasdelivery system.11.2 Select and implement the properly sized test fixture forthe packages to be tested. Verify that the instrument andassociated test fixture have been calibrated fo
29、r the packages tobe tested. The test fixture is too large when the instrument isunable to detect a calibrated control channel or pinhole leak.11.3 Adjust the instrument baseline settings determined incalibration.11.4 Place the package assembly into the test fixture. Makecertain that the package asse
30、mbly is centered in the fixture andthat the lidding side of the package is pointed up toward the testfixture hinged cover and incorporated sealing membrane.NOTE 2The sealing membrane needs to be clean in order to developa good seal with the porous lidding of the package. Laboratory conditionsmay cau
31、se dust or debris to be collected on the sealing membrane. Theseconditions thus warrant frequent inspection and cleaning of the sealingmembrane with a lint-free cloth soaked with a solvent recommended bythe manufacturer of the equipment.11.5 Close the top cover of the test fixture and make certainth
32、at the CO2port makes good contact with the packageassembly.11.6 Start the test.11.7 Note the pass or fail indicator and record results. Setaside any “failed/defective” package for further evaluation.Further evaluation should include re-testing of the package.11.8 Select another package and repeat th
33、e testing process.12. Report12.1 The report shall include the following:12.1.1 A statement indicating that the tests were performedin accordance with ASTM Standard F 2228, except wherenoted.12.1.2 The serial numbers, calibration values and mostrecent calibration dates for all calibration standards u
34、sed.12.1.3 Record the date, time, location, and identification ofthe apparatus and the operator.12.1.4 Record the package type, size, material, product, andtraceable identification numbers.12.1.5 Record the leak rate reject set point as programmedinto the apparatus.12.1.6 Record the number of packag
35、es tested, and thenumber of failed packages.12.1.7 Record the failed packages to be rejected by identi-fying either individual serial numbers or lot numbers.12.1.8 Record the disposition of good packages as well asfailed packages.12.1.9 Copies of any software-generated data sheets, orreports produce
36、d during the testing.13. Precision and Bias13.1 PrecisionA round robin study was conducted in2002, which included three laboratories. Packages with andwithout channels in the seal area and pinholes in the trays weretested for leaks. The equipment used in this interlaboratorystudy was the Pac Guard M
37、odel 500 available from MOCON.13.1.1 Two different package sizes were tested. The largerpackage consisting of a PETE tray and an adhesive coated1073B Tyvek lidding had the approximate outside dimensionsof 129 mm wide by 167 mm long by 20 mm high (5.1 by 6.6by 0.8 in.) with an internal volume of 208
38、mL. The smallerpackage consisted also of a PETE tray and an adhesive coated1073B Tyvek lidding and had the approximate outside dimen-sions of 69 mm wide by 139 mm long by 18 mm high (2.7 by5.5 by 0.7 in.) with an internal volume of 80.7 mL.13.1.2 Three sample packages for each of two sizes (sixpacka
39、ges) 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 aplugged pinhole (no leak).13.1.3 Each sample material was tested at three laboratories,using the same instrumentation. Ea
40、ch package was tested at thetwo possible orientations allowed by the instrument. Two otheroperators subsequently repeated the tests at different times. Agrand total of 324 tests were performed, 216 on materials withleaks and 108 on materials without leaks.13.2 Tables 1-3 represent a summary of the t
41、est data.13.2.1 The results show that none of the 216 tests oncalibrated leaks failed to detect the leak, that is, there were zerofalse negatives. Four of the 108 tests on plugged pinholesresulted in the determination of a leak, that is, a false positive.13.2.2 Four errors occurred at Laboratory 2.
42、It was observedthat dust collected on the sealing membrane and thus propersealing of the porous lidding may not have been accomplished.This condition would allow CO2to flow between the sealingmembrane and the package lidding into the test fixture whereit would be detected and cause the alarm to be t
43、riggered. SeeNote 2 for inspection and cleaning guidelines for the sealingmembrane.13.2.3 Aside from laboratory conditions, it can be arguedthat the instrument tests were independent, and that the numberof defects follows a binomial distribution with probability p oftesting error. An estimate of p i
44、s the error rate, and aconservative confidence interval for p can be determined. Thetables list the upper bound of a 95 % confidence interval for thetrue error rate.TABLE 1 Percent Incorrect by MaterialMaterialTestDeterminationsIncorrectAnalysisPercent (%)Incorrect95 % UpperBoundPackage 324 4 1.2 3.
45、1F 2228 02 (2007)313.2.4 Package size had no effect on the test results.14. Keywords14.1 basal flow; carbon dioxide (CO2) leak testing; flexiblepackaging; infrared CO2sensor; medical packaging; non-destructive testing; package integrity monitoring; packageintegrity test; pass/fail criteria; pass/fai
46、l levels; permeablepackaging; pinhole leaks; porous barrier; porous lids; porouspackaging; rigid thermoformed trays; sealing membrane per-formance; seal integrity monitoring; seal integrity test; sealleaks; sterile integrity tests; trace gas leak testingANNEX(Mandatory Information)A1. LEAK TEST THEO
47、RYA1.1 Placing the lidded package in a test fixture to whichthe infrared sensor is connected initiates the test method. Thismethod does not locate the leak, but instead provides ameasurement of total leakage. The response of the instrumentto any leakage is a non-linear function of the leak (hole) si
48、ze.The sensitivity of this method is a function of trace gasconcentration in the package. It is recommended that the tracegas delivery flow be adjusted to a rate that equals at least twoor more tray volume exchanges per test cycle time, thusyielding close to 90 to 100 % trace gas concentration level
49、swithin the package.A1.2 In this non-destructive test procedure, leaks in medi-cal packages, rigid thermoformed trays with porous lids, aredetected. As shown in Fig. 1, the package with porous liddingis placed in a test fixture where CO2trace gas is delivered tothe outside of the porous lid material through a port in thesealing membrane. The trace gas is forced under pressurethrough the porous lidding into the cavity of the package.Venting, of the excess gas mixture from the package, awayfrom the test fixture is provided.A1.3 Upon initiation of the test cycle,
