1、Designation: F1929 12Standard Test Method forDetecting Seal Leaks in Porous Medical Packaging by DyePenetration1This standard is issued under the fixed designation F1929; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of
2、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 test method defines materials and procedures thatwill detect and locate a leak equal to or greater than a channel
3、formed by a 50 m (0.002 in.) wire in package edge sealsformed between a transparent material and a porous sheetmaterial. A dye penetrant solution is applied locally to the sealedge to be tested for leaks.After contact with the dye penetrantfor a specified time, the package is visually inspected for
4、dyepenetration.1.2 Three dye application methods are covered in this testmethod: injection, edge dip, and eyedropper.1.3 These test methods are intended for use on packageswith edge seals formed between a transparent material and aporous sheet material. The test methods are limited to porousmaterial
5、s which can retain the dye penetrant solution andprevent it from discoloring the seal area for a minimum of 5seconds. Uncoated papers are especially susceptible to leakageand must be evaluated carefully for use with each test method.1.4 These test methods require that the dye penetrantsolution have
6、good contrast to the opaque packaging material.1.5 The values are stated in International System of Units(SI units) and English units. Either is to be regarded asstandard.1.6 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility
7、 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:2F17 Terminology Relating to Flexible Barrier Packaging2.2 ANSI Standards:3Z1.4 Sampling Procedures an
8、d Tables for Inspection byAttributes3. Terminology3.1 wickingthe migration of a liquid into the body of afibrous material. This is distinct from a leak as defined inTerminology F17.3.2 dye penetrantan aqueous solution of a dye and asurfactant designed to penetrate and indicate a defect locationin th
9、e time prior to the onset of wicking which could mask itspresence.3.3 channelrefer to definition in F17.4. Significance and Use4.1 Harmful biological or particulate contaminants mayenter the medical package through leaks. These leaks arefrequently found at seals between package components of thesame
10、 or dissimilar materials. Leaks may also result from apinhole in the packaging material.4.2 It is the objective of this test method to visually observethe presence of channel defects by the leakage of dye throughthem.4.3 This dye penetrant procedure is applicable only toindividual leaks in a package
11、 seal. The presence of a number ofsmall leaks, as found in porous packaging material, whichcould be detected by other techniques, will not be indicated.4.4 There is no general agreement concerning the level ofleakage that is likely to be deleterious to a particular package.However, since these tests
12、 are designed to detect leaks,components that exhibit any indication of leakage are normallyrejected.4.5 These procedures are suitable to verify and locateleakage sites. They are not quantitative. No indication of leaksize can be inferred from these tests. The methods are usuallyemployed as a pass/f
13、ail test.4.6 The dye solution will wick through any porous materialover time, but usually not within the maximum time suggested.1This test method is under the jurisdiction ofASTM Committee F02 on FlexibleBarrier Packagingand is the direct responsibility of Subcommittee F02.40 onPackage Integrity.Cur
14、rent edition approved Nov. 1, 2012. Published January 2013. Originallyapproved in 1998. Last previous edition approved in 2004 as F1929 98(2004).DOI: 10.1520/F1929-12.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual
15、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.,4th Floor, New York, NY 10036.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA
16、 19428-2959. United States1If wicking does occur, it may be verified by observing theporous side of the subject seal area. The dye will havediscolored the surface of the material. Refer to Appendix X1for details on wicking and guidance on the observance of falsepositives.5. Apparatus5.1 Means of bre
17、aching one of the packaging materials suchas a small knife. (Method A)5.2 Dye Dispenser, such as an eyedropper or syringe forinjection of the dye penetrant solution. (Method A)5.3 Dye Solution Container. (Method B)5.4 Scissors or other cutting instrument. (Method B)5.5 Eyedropper or 1 Mil. Pipette.
18、(Method C)5.6 Microscope or optical loop with magnification of 5 to20 (optional for all methods).5.7 Aqueous dye penetrant solution consisting of, byweight:Wetting agent: TRITON X-10040.5 %Indicator dye: Toluidine blue 0.05 %Carrier: Water 99.45 %NOTE 1The solution must remain homogeneous. If precip
19、itate isnoted, the solution must be replaced.5.7.1 If other colored or fluorescent dyes are substituted fortoluidine blue, their precision and bias must be experimentallydetermined.5.7.2 Because of the viscosity of the TRITON X-100, thepreparation of the solution is most easily accomplished by first
20、taring a container with about 10 % of the required amount ofwater 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
21、 Precautions6.1 Injecting dye penetrant into a package with a hypoder-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 dy
22、e penetrantis dispensed using a flexible tube attached to a syringe throughan opening formed with an appropriate cutting instrument.7. Test Specimen7.1 The test specimen shall consist of a complete packageddevice, empty packages, or edge seal samples. Blemished,rejected or dummy products may be used
23、 if they will not affecttest results and are recorded prior to the test.8. Calibration and Standardization8.1 Since these procedures are not quantitative, no calibra-tion is required.9. Sampling9.1 The number of samples tested should be adequate to bepredictive of performance. Caution should be take
24、n wheneliminating samples with defects as this can bias the results.See ANSI ASQC Z1.4.10. Conditioning10.1 Packaging must be free of condensation or any othersource of liquid water. Water already in the seal defects mayrender them undetectable with a dye penetrant. If there is anyindication that th
25、e package has been exposed to any liquid, itmust be thoroughly dried at its typical storage temperaturebefore testing.10.2 If conditioning is required standard conditioning atmo-sphere of 23 6 2C or 73.4 6 3.6F and 50 6 2 % relativehumidity is recommended, for a minimum of 24 hr. prior totesting.11.
26、 Procedure11.1 Method A (Injection Method):11.1.1 Inject sufficient dye penetrant into the package tocover the longest edge to a depth of approximately 5 mm or0.25 in. (see 6.1 for safety precautions).11.1.1.1 When puncturing the packaging to allow injectionof the dye penetrant solution, care should
27、 be taken not topuncture through or damage other package surfaces. Punctur-ing of the package is facilitated if it is done adjacent to adummy device inside the package. The device will provide atenting effect that will separate the two sides of the package,reducing the chance of accidental puncture
28、of both sides.11.1.2 Visually examine the seal area through the transpar-ent side of the package. Observe the package seal area forpenetration of the dye solution across the seal width. Channelsin the seal will be readily detected. Use 5 seconds per side maxas a guide for a 4 sided package. Total ti
29、me should be less thanor equal to 20 seconds. With prolonged exposure wicking ofdye through the porous packaging will color the entire sealmaking defect detection difficult. An optical device with 5 to20 magnification may be used for detailed examination.11.1.3 Rotate the package as necessary to exp
30、ose each sealedge to the dye penetrant solution. Inject additional dye asneeded to insure complete edge exposure.11.2 Method B (Edge Dip Method):11.2.1 Select a container whose length is long enough toaccommodate the longest sealed edge of the package.11.2.2 Pour enough dye into the container to cov
31、er the entirebottom surface to a minimum depth of approximately 36 mmor 0.1250.25 in.11.2.2.1 If the package being tested has excessive materialbeyond the seal, such as a chevron style opening feature, amodification must be made to the package. With a cuttinginstrument, remove the excessive material
32、 along the outsideedge of the chevron seal to a distance of approximately 3 mmor 0.125 in. from the seal, taking care not to cut into the sealarea. Removal of the excess material will allow the dyesolution to come into close proximity to the seal.11.2.3 Lower one of the edges of the package into the
33、 dyesolution so that it briefly touches the dye along the entire edge4TRITON, a registered trademark of Union Carbide, has been found satisfactoryfor this purpose.F1929 122of the seal. This needs to be a brief dip process, just longenough to completely wet the edge.11.2.4 Remove the package in its d
34、ipped orientation, andverify that the entire seal edge has been exposed to the dyesolution. Observe the package seal area, through the transpar-ent side, for penetration of the dye solution across the sealwidth. Use 5 seconds per side max as a guide for a 4 sidedpackage. Total time should be less th
35、an or equal to 20 seconds.11.2.5 An optical device with 5 to 20 magnification maybe used for detailed examination.11.2.6 Repeat edge dip for the remaining seals.11.3 Method C (Eyedropper Method):NOTE 2This method requires the package to have an unsealed areabeyond the outer edge of the seal.11.3.1 P
36、our dye solution into an open container.11.3.2 Using a finger or the end of a paper clip, carefullypush back the extended edge of the porous material away fromthe transparent material.11.3.3 Insert eyedropper or pipette into the dye solution.11.3.4 With the transparent side of the package facing the
37、operator, lay a bead of the dye solution along the top edge ofthe package between the porous and transparent material.Ensure entire edge has been wetted with the dye solution.11.3.5 For small packages slowly rotate the package, whileapplying solution until the entire package seal is exposed to theso
38、lution. Otherwise, apply solution to one side of the packageat a time.11.3.6 Observe the package seal area for penetration of thedye solution across the seal width. Use 5 seconds per side maxas a guide for a 4 sided package. Total time should be less thanor equal to 20 seconds.12. Report12.1 Report
39、the following information:12.1.1 Complete identification of material being tested,including, but not limited to lot number and source of material,date, time, location and operator of test.12.1.2 Any conditioning of the materials.12.1.3 A reference to test method performed: Method A, B,and/or C.12.1.
40、4 Identification of the dye penetrant solution if differ-ent from that specified in section 5.7.12.1.5 Method of visual inspection: aided or unaided.12.1.6 Results:12.1.6.1 Evidence of dye penetration to the opposite side ofthe seal or to the interior of the seal via a defined channel shallbe taken
41、as an indication of the presence of a leakage site.12.1.6.2 Evidence of dye penetration through the porousmaterial through general wetting of the surface (wicking) shallnot be taken as an indication of the presence of a leakage site.12.1.6.3 A qualitative description or sketch of the leakagesites.12
42、.1.6.4 Any deviation from standard.13. Precision and Bias13.1 Injection Method:13.1.1 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
43、 m (0.002in.) 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
44、number ofcorrectly identified defects)/ (the number of test packages).13.1.2 The results show that when using the dye penetranton packages with one side consisting of a porous breathablemembrane, there is more than 95 % confidence that channels inpackage seals will be detected if they are equivalent
45、 in size inthose made with a 50 m (0.002 in.) wire. In this test series,significant reductions in test performance (probability of de-tecting a defect 60 %) were observed with pouches fabricatedwith film on both surfaces and with indicator dyes other thantoluidine blue. Previous testing had shown si
46、gnificantly poorerdetection with other wetting agents. These test results aretherefore specific for this dye and wetting agent formulation.13.1.3 The above P coated 44# paperWith defect 25/25 24/25 22/24No defect 24/24 24/24 25/25Sample 2: Tray with breathable lid; dot coated TYVEKAWith defect 25/25
47、 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 identifie
48、d 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.F1929 123channels) for each of five materials. Every analyst reportedresults to indicate the presence or absence of a
49、 channel. Theresults were tabulated as the number identified correctly, falsepositives, and false negatives; the details are given in ASTMResearch Report No. F02-1032.513.2.2 When combining the edge dip data population of alllabs, the results show that this method provides the correctresponse of detecting channels created by a 50 m wire in seals95 % of the time. The 95 % confidence interval is 93.8 % to96.0 %. The results of correctly identified, false positives andfalse negatives are shown in Tables 2-4.13.2.2.1 When comparing the edge dip labs throughANOVA, la
