1、Designation: F 1929 98 (Reapproved 2004)Standard Test Method forDetecting Seal Leaks in Porous Medical Packaging by DyePenetration1This standard is issued under the fixed designation F 1929; the number immediately following the designation indicates the year oforiginal adoption or, in the case of re
2、vision, 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 defines materials and a procedure thatwill detect and locate a leak equal or gre
3、ater than a channelformed by a 50 m (0.002 in.) wire in package edge sealsformed between a transparent film and a porous sheet material.A dye penetrant solution is applied locally to the seal edge tobe tested for leaks. After contact with the dye penetrant for aspecified time, the package is visuall
4、y inspected for dyepenetration.1.2 This test method is intended for use on packages withedge seals formed between a transparent film and a poroussheet material. This test method is limited to porous materialswhich can retain the dye penetrant solution and prevent it fromdiscoloring the entire seal a
5、rea for a minimum of 20 s.Uncoated papers are especially susceptible to leakage and mustbe evaluated carefully fro use with this test method.1.3 This test method requires that the dye penetrant havegood contrast to the opaque packaging material.1.4 The values stated in SI units are to be regarded as
6、 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 use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the
7、 applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2F 1327 Terminology Relating to Barrier Materials for Medi-cal Packaging2.2 ANSI Standards:3Z1.4 Sampling Procedures and Tables for Inspection byAttributes3. Terminology3.1 wickingThe migration of a liqu
8、id into the body of afibrous material. This is distinct from a leak as defined inTerminology F 1327.3.2 dye penetrantAn aqueous solution of a dye and asurfactant designed to penetrate and indicate a defect locationin the time prior to the onset of wicking which could mask itspresence.3.3 channelA sm
9、all continuous open passage across thewidth of a package seal through which microorganisms couldpass. It is the objective of this test method to visually observethe presence of these defects by the leakage of dye throughthem.4. Significance and Use4.1 Harmful biological or particulate contaminants m
10、ayenter the device through leaks. These leaks are frequentlyfound at seals between package components of the same ordissimilar materials. Leaks may also result from a pinhole inthe packaging material.4.2 This dye penetrant procedure is applicable only toindividual leaks in a package seal. The presen
11、ce of a number ofsmall leaks, as found in porous packaging material, whichcould be detected by other techniques, will not be indicated.4.3 There is no general agreement concerning the level ofleakage that is likely to be deleterious to a particular package.However, since these tests are designed to
12、detect leakage,components that exhibit any indication of leakage are normallyrejected.4.4 Since leaks may change in size with different ambientconditions, comparisons between test stations are not conclu-sive. Therefore this method is usually employed as a go, no-gotest.1This test method is under th
13、e jurisdiction of ASTM Committee F02 on FlexibleBarrier Materials and is the direct responsibility of Subcommittee F02.40 onPackage Integrity.Current edition approved June 1, 2004. Published June 2004. Originallyapproved in 1998. Last previous edition approved in 1998 as F 1929 98.2For referenced AS
14、TM 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 onthe ASTM website.3Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4t
15、h Floor, New York, NY 10036.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.4.5 The dye solution will wick through any porous materialover time, but usually not within the maximum time suggested.If wicking does occur, it may be verif
16、ied by observing theporous side of the subject seal area. The dye will havediscolored the surface of the material.4.6 When puncturing the packaging to allow injection of thedye penetrant solution, care should be taken not to punctureother package surfaces. Puncturing of the package is facilitatedif
17、it is done adjacent to a dummy device inside the package.The device will provide a tenting effect that will separate thetwo sides of the package, reducing the chance of accidentalpuncture of both sides.5. Apparatus5.1 Means of breaching one of the packaging materials suchas a small knife.5.2 Dye Dis
18、penser, such as an eyedropper or syringe forinjection of the dye penetrant solution.5.3 Microscope or optical loop with magnification of 53 to203.5.4 Fresh aqueous dye penetrant solution consisting of, byweight:Wetting agent: TRITON X-10040.5 %Indicator dye: Toluidine blue 0.05 %5.5 Other colored or
19、 fluorescent dyes may be substituted fortoluidine blue but their precision and bias must be experimen-tally determined.5.6 Because of the viscosity of the TRITON X-100 thepreparation of the solution is most easily accomplished by firsttaring a container with about 10 % of the required amount ofwater
20、 on a scale. The appropriate amount of TRITON X-100 isadded to the water by weight and the mixture stirred or shaken.Once the TRITON X-100 is dispersed, the remaining water canthen be added, followed by the toluidine blue dye.6. Safety Precautions6.1 Injecting dye penetrant into a package with a hyp
21、oder-mic needle and syringe is a common method for performingthis test. This practice can result in puncture of the skin with acontaminated needle and is therefore not recommended. Be-cause of this hazard, it is recommended that the dye penetrantbe dispensed using a flexible tube attached to a syrin
22、ge throughan opening formed with an appropriate cutting instrument.7. Test Specimen7.1 The test specimen shall consist of a complete packageddevice if the test will be used as a quality control method.Blemished or rejected products may be used if the defect willnot affect test results and is recorde
23、d prior to the test.7.2 Dummy test items, empty packages, or edge sealsamples may be used for process control, product acceptance,or material development testing.8. Calibration and Standardization8.1 These procedures are suitable for use on selected partsduring receiving inspection or to verify and
24、locate leakage sitesfor production control. They are not quantitative. No indicationof leak size can be inferred from the test.9. Conditioning9.1 Packaging must be free of condensation or any othersource of liquid water. Water already in the seal defects mayrender them undetectable with a dye penetr
25、ant. If there is anyindication that the package has been exposed to any liquid, itmust be thoroughly dried at its typical storage temperaturebefore testing.9.2 Test specimens shall be conditioned prior to testing.When no specific conditioning requirements are given, andpackaging materials are moistu
26、re sensitive, a standard condi-tioning atmosphere of 23 6 2C (73.4 6 3.6F) and 50 6 2%relative humidity is recommended, for a minimum of 24 h priorto testing.10. Procedure10.1 Cleaning of packaging prior to dye penetrant applica-tion is unnecessary.10.2 Inject sufficient dye penetrant into the packa
27、ge to coverthe longest edge to a depth of approximately 5 mm (0.25 in.).Allow the dye penetrant solution to remain in contact with theseal edge for a minimum of 5 s and a maximum of 20.Channels will be detected within this time period but beyond20 s, wicking of dye through the porous packaging will
28、colorthe entire seal.10.3 Rotate the package as necessary to expose each sealedge to the dye penetrant solution. Inject additional dye asneeded to insure complete edge exposure.10.4 Visually examine the seal area through the transparentside of the package. Channels in the seal will be readilyapparen
29、t without magnification, as the dye will rapidly wickinto the area adjacent to the channel, making a much largerstain than the actual channel size.An optical device with 73 to203 magnification may be used for detailed examination.11. Report11.1 Report the following information:11.1.1 A reference to
30、this test method,11.1.2 Identification of the dye penetrant,11.1.3 Method of inspection, and11.1.4 Results:11.1.4.1 Evidence of dye penetration to the opposite side ofthe seal or to the interior of the seal via a defined channel shallbe taken as the indication of the presence of a leakage site.11.1.
31、4.2 Evidence of dye penetration through the porousmaterial through general wetting of the surface (wicking) shallnot be taken as the indication of the presence of a leakage site.11.1.4.3 A qualitative description or sketch of the leakagesites.4TRITON, a registered trademark of Union Carbide, has bee
32、n found satisfactoryfor this purpose.F 1929 98 (2004)212. Precision and Bias12.1 Between June 1997, and March 1998 test packagesfrom four manufacturers were examined using this method bythree independent laboratories. Defects were intentionallycreated in the package seals by placing wires of 50 m (0
33、.002in.) diameter in the seal area. When the wires were removed achannel approximately the size of the wire was created in theseal. For each specimen set, 50 packages were produced, 25with wire created defects and 25 controls with no artificialdefects. The results are shown in Table 1 as (the number
34、 ofcorrectly identified defects)/(the number of test packages).12.2 The results show that when using the dye penetrant asspecified in this test methodology on packages with one sideconsisting of a porous breathable membrane there is better than95 % confidence that channels in package seals, equivale
35、nt insize in those made with a 50 m (0.002 in.) wire will bedetected. In this test series, significant reductions in testperformance (probability of detecting a defect 60 %) wereobserved with pouches fabricated with film on both surfacesand with indicator dyes other than toluidine blue. Previoustest
36、ing had shown significantly poorer detection with otherwetting agents. These test results are therefore specific for thisdye and wetting agent formulation.13. Keywords13.1 Dye penetrant; flexible packaging; porous packaging;seal leaksASTM International takes no position respecting the validity of an
37、y patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to rev
38、ision 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
39、 comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyr
40、ighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org
41、 (e-mail); or through the ASTM website(www.astm.org).TABLE 1 Results on Testing Seals with Channels GeneratedUsing 50 m (0.002 in.) WiresTest Site 1 2 3Sample 1: Breathable pouch; coated 44# paperWith defect 25/25 24/25 22/24No defect 24/24 24/24 25/25Sample 2: Tray with breathable lid; dot coated T
42、YVEKAWith defect 25/25 25/25 24/25No defect 25/25 25/25 25/25Sample 3: Breathable pouch; coated TYVEKWith defect 25/25 25/25 24/24No defect 23/25 25/25 25/25Sample 4: Breathable pouch; dot coated TYVEKWith defect 24/25 25/25 25/25 25/25BNo defect 25/25 25/25 25/25 25/25SummaryDefective No DefectNumber correctly identified 318 321Total tested 323 323Percent correctly identified 98 % 99 %ATYVEK, a registered trademark of DuPont, has been found satisfactory for thispurpose.BTested at manufacturing site.F 1929 98 (2004)3
