1、Designation: F2227 02 (Reapproved 2007)F2227 13Standard Test Method forNon-Destructive Detection of Leaks in Non-sealed andEmpty Medical Packaging Trays by CO2 Tracer Gas Method1This standard is issued under the fixed designation F2227; the number immediately following the designation indicates the
2、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 detects pinhole lea
3、ks in trays, as small as 50 m (0.002 in.) in diameter, or equivalentlysized cracks, subject to trace gas concentration in the tray, tray design and manufacturing tolerances.1.2 The values stated in SI units are to be regarded as standard units. Values in parentheses are for information only.1.3 This
4、 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 health practices and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.
5、1 ASTM Standards:2D996 Terminology of Packaging and Distribution EnvironmentsF1327 Terminology Relating to Barrier Materials for Medical Packaging (Withdrawn 2007)33. Terminology3.1 General Term DefinitionsFor definitions used in this test method, see Terminologies D996 and F1327, Sections 3.3.2 Def
6、initions of Terms Specific to This Standard:3.2.1 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 packagingtrays. The test method provid
7、es a qualitative (accept/reject) inspection method to evaluate trays for pinholes and cracks. Furtherinformation on the “Leak Test Theory” may be found in Annex A1.5. Significance and Use5.1 Harmful biological or particulate contaminants may enter the package through imperfections such as pinholes o
8、r cracks intrays.5.2 After initial instrument set-up and calibration, the operations of individual tests and test results do not need operatorinterpretation.5.3 Leak test results that exceed the permissible threshold setting are indicated by audible or visual signal responses, or both,or by other me
9、ans.5.4 This non-destructive test method may be performed in either laboratory or production environments and may be undertakenon either a 100 % or a statistical sampling basis. This test method, in single instrument use and current implementation, may notbe fast enough to work on a production packa
10、ging line, but is well suited for statistical testing as well as package developmentaldesign work.1 This test method is under the jurisdiction of ASTM Committee F02 on Flexible Barrier Packaging and is the direct responsibility of Subcommittee F02.40 on PackageIntegrity.Current edition approved Apri
11、l 1, 2007Aug. 1, 2013. Published May 2007September 2013. Originally approved in 2002. Last previous edition approved in 20022007 asF2227 02.F2227 02 (2007). DOI: 10.1520/F2227-02R07.10.1520/F2227-13.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service
12、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 standard is referenced on www.astm.org.This document is not an ASTM standard and is intended only to provide the us
13、er 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 recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard a
14、s 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 States16. Apparatus6.1 Non-destructive Trace Gas Leak Detection ApparatusThe apparatus test fixture consists of three major element
15、s and isshown in Fig. 1.6.2 Sealing MembraneThe purpose of the membrane is to seal off the tracer gas transmission out of the top of the open tray.6.3 Control TraysCalibrated pinholes, or leaks, constructed in control trays for instrument calibration as well as for testprocedure verification.6.4 Tes
16、t 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. Theinstrument must be operated in an environment as described in the instru
17、ments user manual.8. Reagents and Materials8.1 CO2 Trace Gas Cylinder and RegulatorAcylinder of “Commercial” or “Bone Dry” grade carbon dioxide with a minimumof 206.84-kPa (30-psi) pressure is required for calibration and testing.8.2 Sealing MembraneThe sealing membrane must exhibit the correct plia
18、bility and tackiness in order to form a gas-tightbond without leaving a residue on the tray-sealing surface after removal from the test fixture.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
19、 is allowed to displace oxygen. Thus it isrecommended that the spent carbon dioxide 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 proced
20、ure is used for overall systemcheckout, as well as to establish an initial reference profile for simulated pinhole leaks, and to determine test limits for eachdifferent tray geometry to be tested using a specific test fixture. The calibration procedure is performed to establish the sensitivitysettin
21、g of the instrumentation. It is expected that the calibration procedures be carried out frequently; typically, at least one or moretimes a day, preferably at the beginning of every shift.10.2 Refer to the instrument manufacturers operating instructions regarding preparation of Calibration Standards,
22、 Conditioningof Calibration Trays and Instrument Calibration used in establishing baseline settings.FIG. 1 Schematic of Test Fixture and Test TrayF2227 13211. Procedure11.1 Verify that sufficient CO2 trace gas is available for the tests. Monitor the trace gas supply and functionality of the gasdeliv
23、ery system.11.2 Select and implement the properly sized test fixture for the trays to be tested. Verify that the instrument and associated testfixture have been calibrated for the trays to be tested. The test fixture is too large when the instrument is unable to detect acalibrated control pinhole le
24、ak.11.3 Adjust the instrument baseline settings determined in calibration.11.4 Place the tray to be tested into the test fixture making certain that the tray is centered in the fixture and that good sealingcontact is made between the tray flange and the fixture incorporated sealing.NOTE 1The sealing
25、 membrane needs to be clean in order to develop a good seal with the sealing flange of the tray. Laboratory conditions may causedust or debris to be collected on the sealing membrane. These conditions thus will warrant frequent inspection and cleaning of the sealing membrane witha lint-free cloth so
26、aked with a solvent recommended by the manufacturer of the equipment.11.5 Close the top cover of the test fixture.11.6 Start the test.11.7 Note the pass or fail indicator and record results. Set aside any “failed/defective” trays for further evaluation. Furtherevaluation should include re-testing of
27、 the tray.11.8 Select another tray 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 F2227, except where noted.12.1.2 The serial numbers, calibration values and most recent
28、 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 tray type, size, material, product, and traceable identification numbers.12.1.5 Record the leak rate reject set point as programmed int
29、o the apparatus.12.1.6 Record the number of trays tested, and the number of failed trays.12.1.7 Record the failed trays to be rejected by identifying either individual serial numbers or lot numbers.12.1.8 Record the disposition of good trays as well as failed trays.12.1.9 Copies of any software-gene
30、rated data sheets, or reports produced during the testing.13. Precision and Bias13.1 PrecisionAround robin study was conducted in 2002, which included three laboratories. Trays with and without pinholeleaks were tested for leaks. The equipment used in this interlaboratory study was the Pac Guard Mod
31、el 500 available fromMOCON.13.1.1 Two different tray sizes were tested. The large PETE trays had the approximate outside dimensions of 129 mm wide by167 mm long by 20 mm high (5.1 by 6.6 by 0.8 in.) with an internal volume of 208 mL. The small PETE trays had the approximateoutside dimensions of 69 m
32、m wide by 139 mm long by 18 mm high (2.7 by 5.5 by 0.7 in.) with an internal volume of 80.7 mL.13.1.2 Three sample trays for each of two sizes (six trays) had a 50 m (0.002 in.) calibrated pinhole (leak), and six similar trayshad a plugged pinhole (no leak).13.1.3 Each sample material was tested at
33、three laboratories, using the same instrumentation. Each tray was tested at the twopossible orientations allowed by the instrument.Two other operators subsequently repeated the tests at different times.Agrand totalof 216 tests were performed, 108 on materials with leaks and 108 on materials without
34、leaks.13.2 Tables 1-3 represent a summary of all test data.TABLE 1 Percent Incorrect by MaterialMaterial TestDeterminations IncorrectAnalysis Percent (%)Incorrect 95 % UpperBoundTray 216 0 0.0 1.7TABLE 2 Percent Incorrect by LaboratoryLab TestDeterminations IncorrectAnalysis Percent (%)Incorrect 95
35、% UpperBound1 72 0 0.0 5.02 72 0 0.0 5.03 72 0 0.0 5.0F2227 13313.2.1 The results show that none of the 108 tests on calibrated leaks failed to detect the leak, that is, there were zero falsenegatives. There were also no false positives.13.2.2 Aside from laboratory conditions, it can be argued that
36、the instrument tests were independent, and that 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 f
37、or the true error rate.13.2.3 Tray size had no effect on the test results.13.3 BiasThe bias for this test method has not been determined because there is no known standard reference available.14. Keywords14.1 carbon dioxide (CO2) leak testing; flexible packaging; infrared CO2 sensor; medical package
38、 integrity test; non-destructivetesting; package integrity monitoring; pass/fail criteria; permeable packaging; pinhole leaks; porous packaging; sealing membraneperformance; sterile integrity tests; trace gas leak testing; trays pass/fail levelsTABLE 3 Percent Incorrect by Defect TypeDefect Type Tes
39、tDeterminations IncorrectAnalysis Percent (%)Incorrect 95 % UpperBoundPlugged pinhole 108 0 0.0 3.450 m pinhole 108 0 0.0 3.4F2227 134ANNEX(Mandatory Information)A1. LEAK TEST THEORYA1.1 Placing the unlidded tray in a test fixture to which the infrared sensor is connected initiates the test method.
40、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 tray. It isrecommended that the trac
41、e gas delivery flow be adjusted to a rate that equals at least two or more tray volume exchanges per testcycle time, thus yielding close to 90 to 100 % trace gas concentration levels within the tray.A1.2 In this test procedure, pinhole leaks or cracks in trays are detected. As shown in Fig. 1, the t
42、ray is placed in a test fixturesuch that a good, vacuum tight contact is made between the tray flange and associated fixture sealing (sealing membrane). CO2trace gas is then introduced into the sealed cavity of the tray.A1.3 Upon initiation of the test cycle, the tray is flushed with CO2 trace gas a
43、t a predetermined flow rate.The internal tray pressureof CO2 is generally set between 0.25 and 0.75 kPa (0.0363 to 0.1088 psi or 1 to 3 in. of water H2O column). During thisflushing/soaking cycle, room air is drawn through the test fixture at a low vacuum of approximately 0.0249 kPa (0.00361 psi or0
44、.1 in. of H2O column) and channeled past the infrared detection sensor. Near the end of the flushing/soaking cycle, a solenoidvalve is energized causing the room air drawn flow to be cut off, thus producing an ambient pressure within the capture volumeof the test fixture. If the tray has a pinhole o
45、r crack then some carbon dioxide will leak out of the tray and accumulate in the capturevolume of the test fixture.A1.4 At the end of the test period, the solenoid valve reverts back to its initial (open) position. This permits room air to again flowto the test fixture chamber. A pump then flushes t
46、he room air through the capture volume, which in turn picks up any CO2 thatmay have escaped out of the tray and pulls it through the infrared sensing chamber. If the carbon dioxide concentration in thecapture volume is significantly higher than that of the room air, the carbon dioxide alarm will be
47、activated. In order to reducepotential false positive signal responses from the instrumentation, it is recommended that the ambient carbon dioxide levels notfluctuate since varying levels of carbon dioxide may affect the sensitivity of the system. Thus, it is highly recommended that theexhausted CO2
48、 be naturally vented, through appropriate piping, away from the test area.ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity
49、of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn.Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If yo
