1、Designation: F 2096 04Standard Test Method forDetecting Gross Leaks in Medical Packaging by InternalPressurization (Bubble Test)1This standard is issued under the fixed designation F 2096; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revi
2、sion, 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 test method covers the detection of gross leaks inmedical packaging. Method sensitivity is dow
3、n to 250 m withan 81 % probability (see Section 11). This test method may beused for tray and pouch packages.1.2 The sensitivity of this test method has not been evalu-ated for use with porous materials other than spunbondedpolyolefin or with nonporous packaging.1.3 This test method is destructive i
4、n that it requires entryinto the package to supply an internal air pressure1.4 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for informationonly.1.5 This standard does not purport to address all of thesafety concerns, if any, associated with its
5、 use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 1898 Practice for Sampling of Plastics3F 1327 Terminology Relating to
6、Barrier Materials for Medi-cal Packaging3. Terminology3.1 DefinitionsGeneral terms relating to barrier materialsfor medical packaging are found in Terminology F 1327.3.2 Definitions of Terms Specific to This Standard:3.2.1 breathing point pressure, npressure at which perme-ation of air through the p
7、orous material begins.44. Summary of Test Method4.1 The package is inflated underwater to a predeterminedpressure. The package is then observed for a steady stream ofair bubbles indicating a failure area.4.2 The sensitivity of this test method is dependent on thedifferential pressure and method of p
8、ressurization. Establish-ment of a test pressure for each package material/size is criticalfor obtaining repeatable results (see Annex A1 for the proce-dure on establishing test pressure). Inadequate pressurizationof the package can significantly reduce the sensitivity of thistest method. Higher dif
9、ferential pressures will increase the testsensitivity. However, excessive pressurization of the packagemay rupture seals or cause misinterpretation of bubble patternsemanating from porous packaging. This may result in anerroneous conclusion regarding the presence or absence ofpackage defects. While
10、not required, use of a bleed-off controlvalve in line with the pressure monitoring device, will aid instabilizing the test pressure, and help eliminate excessivepressurization of the package (see Fig. 1).4.3 Two different test methods are presented for the testingof porous and nonporous packaging. T
11、he key differencebetween the test methods (as described in Annex A1)isinallowing time for the water to saturate the porous material.5. Significance and Use5.1 The internal pressurization test method provides a prac-tical way to examine packages for gross leaks, which mayrender the product non-steril
12、e.5.2 This test method is extremely useful in a test laboratoryenvironment where no common package material/size exists.5.3 This test method may apply to very large or longpackages, which do not fit into any other package integrity testmethod apparatus.5.4 This test method may be used as a means to
13、evaluatepackage integrity. Package integrity is crucial to consumer1This test method is under the jurisdiction of ASTM Committee F02 on FlexibleBarrier Materials and is the direct responsibility of Subcommittee F02.40 onPackage Integrity.Current edition approved April 1, 2004. Published June 2004. O
14、riginallyapproved in 2001. Last previous edition approved in 2002 as F 2096 02e1.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page
15、 onthe ASTM website.3Withdrawn.4All porous packaging by definition will permit the passage of air. At a giveninternal pressure it will therefore exhibit an emanating stream of air bubblesdependent on the pore size. A stream of bubbles identified at a lower internalpressure than the breathing pressur
16、e point may indicate a defect in the packaging.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.safety since heat sealed packages are designed to provide acontamination free and sterile environment to the product.6. Apparatus6.1 Press
17、ure Delivery System, with pressure monitoringgage, and bleed-off control valve, capable of delivering air at apressure of 0-50 mbar (0-20 in. H2O).6.2 Device for Puncturing Package, (for example, smallslotted screwdriver or other appropriate device) to allowinsertion of air source and pressure monit
18、oring device.6.3 Water Container, adequate to cover the test specimenwith approximately one (1) in. of H2O.7. Sampling7.1 The number of test specimens shall be chosen to permitan adequate determination of representative performance.Practice D 1898 provides guidance for test speciman selection.8. Con
19、ditioning8.1 No special conditioning of the specimen is required.9. ProcedureNOTE 1The establishment of a test pressure in accordance withAnnex A1 must be performed prior to initiating the test procedure.9.1 Test Method AProcedure for Nonporous Packaging:9.1.1 Create a hole in the package using a pu
20、ncturing device(for example, small slotted screwdriver or other appropriatedevice) for inserting the air source and pressure monitor intothe control sample. Create the hole as close to the center of thepackage as possible. The hole size should allow insertion of theair source and pressure monitor wi
21、th minimal air leakage. Usetape or a rubber disk as a septum over the puncture site to sealthe insertion site if necessary.9.1.2 Insert the air source and pressure monitor into the testspecimen. Submerge the package under water approximatelyone (1) in. Start airflow into the package.NOTE 2It may be
22、helpful to use a fixture to keep the entire packagesubmerged at the proper depth.9.1.3 Adjust the airflow and bleed-off valve as necessary toslowly inflate the package to a value equal to or greater than theminimum test pressure as established in accordance withAnnex A1. Adjust the bleed-off valve a
23、nd pressure regulator asnecessary to maintain constant pressure.9.1.4 Thoroughly inspect the package for a constant streamof bubbles indicating a specific area of failure (seal channels,pinholes, cracks, tears, and so forth). Inspection time will varydepending on package size.FIG. 1 Sample Test Appa
24、ratusF20960429.1.5 Remove the package from water and mark any ob-served area(s) of failure.9.2 Test Method BProcedure for Porous Packaging:9.2.1 Apply blocking agent to samples if required in accor-dance with A1.1.2.4.9.2.2 Create a hole in the package using a puncturing device(for example, small sl
25、otted screwdriver or other appropriatedevice) for inserting the air source and pressure monitor intothe control sample. Create the hole as close to the center of thepackage as possible. The hole size should allow insertion of theair source and pressure monitor with minimal air leakage. Usetape or a
26、rubber disk as a septum over the puncture site to sealthe insertion site if necessary.9.2.3 Insert the air source and pressure monitor into thepackage. Submerge the package under water approximately 1in. and hold for a minimum of 5 s. Start the airflow into thepackage.NOTE 3It may be helpful to use
27、a fixture to keep the entire packagesubmerged at the proper depth.9.2.4 Adjust the airflow and bleed-off valve as necessary toslowly inflate the package to a value equal to or greater than theminimum test pressure as established in accordance withAnnex A1. Adjust the bleed-off valve and pressure reg
28、ulator asnecessary to maintain constant pressure.9.2.5 Thoroughly inspect the package for a constant streamof bubbles indicating a specific area of failure (seal channels,pinholes, cracks, tears, and so forth). Inspection time will varydepending on package size.9.2.6 Remove the package from the wate
29、r and mark anyobserved area(s) of failure.10. Report10.1 Report the following information:10.1.1 Date, time, location, and operators name.10.1.2 Package type, size, material, and traceable identifi-cation numbers.10.1.3 Description of package preparation including pres-ence of any product in package
30、.10.1.4 Established defect size used to establish the testsensitivity, test pressure, and use of any blocking agent.10.1.5 Number of test packages, approximate inspectiontime per package, number of packages exhibiting leaks, andlocation of each leak.11. Precision and Bias11.1 A round-robin study was
31、 conducted in 2000, whichincluded 5 laboratories, two package types, and two defecttypes. The defects consisted of a channel through the seal areaon the pouch samples and a puncture through the porousmaterial, on both the tray and pouch samples.All defect samplegroups were created with a 125-m (0.00
32、5 in.) and 250-m(0.010 in.) wire. The first package type consisted ofa4by6-in.heat-sealed pouch, made from a combination clear film anduncoated Tyvek.5The second package type consisted ofa3by5-in. thermoformed polycarbonate tray, heat-sealed with anadhesive zone coated Tyvek. The negative controls c
33、onsisted ofthe same packages produced with no defects. For each speci-men set, 15 samples were produced, 10 with defects, and 5controls with no defect. The results are presented in Table 1and the corresponding graph in Fig. 2.11.2 The analysis of the testing process is by means oflogistic regression
34、. The computations were performed in SAS,version 8.1. The y-axis is the probability of rejecting a part, andthe x-axis is the nominal defect size. The results of this analysisindicate that there is an 81 % probability of rejecting a packagewith a defect size of 250 m. There is also an 11 % probabili
35、tyof rejecting a package with no defects.12. Keywords12.1 bubble test; internal pressurization; package integrity5Tyvek is a registered trademark of Dupont and has been found satisfactory forthis purpose.TABLE 1 Percent Correct by Laboratory and Defect TypeDefect TypePouch TrayLaboratoryNoDefects125
36、-mChannel250-mChannel125-mPuncture250-mPunctureNoDefects125-mPuncture250-mPuncturePercent Correctby Laboratory1 100 100 90 60 80 100 40 90 82.502 100 70 90 50 60 90 10 100 71.253 80 20 80 60 80 90 60 80 68.754 100 70 90 0 0 100 60 100 65.005 80 20 100 0 30 100 20 90 55.00Percent Correctby Defect92 5
37、6 90 34 50 96 38 92F2096043ANNEX(Mandatory Information)A1. ESTABLISHMENT OF TEST PRESSUREA1.1 This test method uses a control sample with a knowndefect for establishing the test pressure for the packagematerial/size.Aknown defect is created in the package surface.The package is submerged in water an
38、d inflated to a pressurewhere air bubbles are observed emanating from the defect. Thisis considered the minimum test pressure for the given package.Inadequate pressurization of the package can significantlyreduce the sensitivity of the test method. Higher differentialpressures will increase the test
39、 sensitivity. However, excessivepressurization of the package may rupture seals or causemisinterpretation of bubble patterns emanating from porouspackaging. This may result in an erroneous conclusion regard-ing the presence or absence of package defects.During feasibility studies, it was noted that
40、the pressure atwhich the permeation of air through the porous material began(breathing point pressure), was significantly less when apositive airflow was introduced into the package before sub-mersion. A study was performed to determine the effects ofwater permeation on the breathing point pressure
41、of the Tyvek.A positive airflow was introduced into a test sample beforesubmersion. When the package was submerged in water, at adepth of 1 in., the breathing point pressure was recorded atapproximately 4 to 5 in. H2O. A test sample was thensubmerged in water, at a depth of 1 in., for a minimum of 5
42、 s,prior to the airflow being introduced into the package. Thebreathing point pressure increased to approximately 9 in. H2O.The test was then repeated with a known defect produced in thepackage. The pressure at which the defect was observed was 5in. H2O. Introduction of an airflow prior to submersio
43、n, or aftersubmersion, did not effect the pressure at which the defect wasobserved. However, due to the permeation of air through theTyvek, the defect could not be consistently detected when theairflow was started prior to submersion.A1.1.1 Establishment of Test Pressure for Nonporous Pack-agingA1.1
44、.1.1 Create a known defect in the control sample to thedesired sensitivity for the test method (defect not to exceed 250microns). Circle the location of the defect with a felt pen.Record the defect size for reporting purposes.A1.1.1.2 Create a hole in the package using a puncturingdevice (for exampl
45、e, a small slotted screwdriver) for insertingthe air source and pressure monitor into control sample. Createthe hole as close to the center of the package as possible. Thehole size should allow insertion of the air source and pressuremonitor with minimal air leakage. Use tape or a rubber disk asa se
46、ptum over the puncture site to seal the insertion site ifnecessary. The location of the hole should not interfere with thedefect created in A1.1.1.1.A1.1.1.3 Insert the air source and pressure monitor into thecontrol sample. Submerge the control sample under waterapproximately 1 in. Start the airflo
47、w into the control sample.A1.1.1.4 Adjust the airflow and bleed-off valve as neces-sary, to gradually inflate the control sample to the point wherethe defect manifests itself. Record the pressure reading. Thispressure will be the minimum test pressure. Higher differentialpressures will increase the
48、test sensitivity. However, excessivepressurization of the package may rupture seals.FIG. 2 Probability of Rejection-Combined Laboratory ResultsF2096044A1.1.2 Establishment of Test Pressure for Porous MaterialPackagingA1.1.2.1 Create a known defect in the control sample to thedesired sensitivity for
49、the test method (defect not to exceed 250microns). Circle the location of the defect with a felt pen.Record the defect size for reporting purposes.A1.1.2.2 Create a hole in the package using a puncturingdevice (for example, a small slotted screwdriver) for insertingthe air source and pressure monitor into the control sample.Create the hole as close to the center of the package aspossible. The hole size should allow insertion of the air sourceand pressure monitor with minimal air leakage. Use tape or arubber disk as a septum over the puncture site to seal theinserti
