1、Designation: F1929 12F1929 15Standard 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
2、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 test method defines materials and procedures that will detect and locate a leak equal to or greater than
3、a channel formedby a 50 m (0.002 in.) wire in package edge seals formed between a transparent material and a porous sheet material. A dyepenetrant solution is applied locally to the seal edge to be tested for leaks.After contact with the dye penetrant for a specified time,the package is visually ins
4、pected for dye penetration.1.2 Three dye application methods are covered in this test method: injection, edge dip, and eyedropper.1.3 These test methods are intended for use on packages with edge seals formed between a transparent material and a poroussheet material. The test methods are limited to
5、porous materials which can retain the dye penetrant solution and prevent it fromdiscoloring the seal area for a minimum of 5 seconds. Uncoated papers are especially susceptible to leakage and must be evaluatedcarefully for use with each test method.1.4 These test methods require that the dye penetra
6、nt solution have 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 as standard.1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It
7、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 Documents2.1 ASTM Standards:2F17 Terminology Relating to Flexible Barrier Packaging2.2 ANSI Standards:3Z1.4 Sampl
8、ing Procedures and Tables for Inspection by Attributes3. Terminology3.1 wickingthe migration of a liquid into the body of a fibrous material. This is distinct from a leak as defined in TerminologyF17.3.2 dye penetrantan aqueous solution of a dye and a surfactant designed to penetrate and indicate a
9、defect location in the timeprior to the onset of wicking which could mask its presence.3.3 channelrefer to definition in F17.4. Significance and Use4.1 Harmful biological or particulate contaminants may enter the medical package through leaks. These leaks are frequentlyfound at seals between package
10、 components of the same or dissimilar materials. Leaks may also result from a pinhole in thepackaging material.4.2 It is the objective of this test method to visually observe the presence of channel defects by the leakage of dye through them.1 This test method is under the jurisdiction of ASTM Commi
11、ttee F02 on Flexible Barrier Packagingand is the direct responsibility of Subcommittee F02.40 on PackageIntegrity.Current edition approved Nov. 1, 2012Oct. 1, 2015. Published January 2013December 2015. Originally approved in 1998. Last previous edition approved in 20042012as F1929 98F1929 12.(2004).
12、 DOI: 10.1520/F1929-12.10.1520/F1929-15.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.3 Available from Amer
13、ican National Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible t
14、o adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Con
15、shohocken, PA 19428-2959. United States14.3 This dye penetrant procedure is applicable only to individual leaks in a package seal. The presence of a number of smallleaks, as found in porous packaging material, which could be detected by other techniques, will not be indicated.4.4 There is no general
16、 agreement concerning the level of leakage that is likely to be deleterious to a particular package.However, since these tests are designed to detect leaks, components that exhibit any indication of leakage are normally rejected.4.5 These procedures are suitable to verify and locate leakage sites. T
17、hey are not quantitative. No indication of leak size canbe inferred from these tests. The methods are usually employed as a pass/fail test.4.6 The dye solution will wick through any porous material over time, but usually not within the maximum time suggested. Ifwicking does occur, it may be verified
18、 by observing the porous side of the subject seal area. The dye will have discolored thesurface of the material. Refer to Appendix X1 for details on wicking and guidance on the observance of false positives.5. Apparatus5.1 Means of breaching one of the packaging materials such as a small knife. (Met
19、hod A)5.2 Dye Dispenser, such as an eyedropper or syringe for injection 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. (Method C)5.6 Microscope or optical loop with magnification of
20、5 to 20 (optional for all methods).5.7 Aqueous dye penetrant solution consisting of, by weight:Wetting agent: TRITON X-1004 0.5 %Indicator dye: Toluidine blue 0.05 %Carrier: Water 99.45 %NOTE 1The solution must remain homogeneous. If precipitate is noted, the solution must be replaced.5.7.1 If other
21、 colored or fluorescent dyes are substituted for toluidine blue, their precision and bias must be experimentallydetermined.5.7.2 Because of the viscosity of the TRITON X-100, the preparation of the solution is most easily accomplished by first taringa container with about 10 % of the required amount
22、 of water on a scale. The appropriate amount of TRITON X-100 is added tothe water by weight and the mixture stirred or shaken. Once the TRITON X-100 is dispersed, the remaining water can then beadded, followed by the toluidine blue dye.6. Safety Precautions6.1 Injecting dye penetrant into a package
23、with a hypodermic needle and syringe is a common method for performing this test.This practice can result in puncture of the skin with a contaminated needle and is therefore not recommended. Because of thishazard, it is recommended that the dye penetrant is dispensed using a flexible tube attached t
24、o a syringe through an opening formedwith an appropriate cutting instrument.7. Test Specimen7.1 The test specimen shall consist of a complete packaged device, empty packages, or edge seal samples. Blemished, rejectedor dummy products may be used if they will not affect test results and are recorded
25、prior to the test.8. Calibration and Standardization8.1 Since these procedures are not quantitative, no calibration is required.9. Sampling9.1 The number of samples tested should be adequate to be predictive of performance. Caution should be taken wheneliminating samples with defects as this can bia
26、s the results. See ANSI ASQC Z1.4.10. Conditioning10.1 Packaging must be free of condensation or any other source of liquid water. Water already in the seal defects may renderthem undetectable with a dye penetrant. If there is any indication that the package has been exposed to any liquid, it must b
27、ethoroughly dried at its typical storage temperature before testing.10.2 If conditioning is required standard conditioning atmosphere of 23 6 2C or 73.4 6 3.6F and 50 6 2 % relative humidityis recommended, for a minimum of 24 hr. prior to testing.4 TRITON, a registered trademark of Union Carbide, ha
28、s been found satisfactory for this purpose.F1929 15211. Procedure11.1 Method A (Injection Method):11.1.1 Inject sufficient dye penetrant into the package to cover the longest edge to a depth of approximately 5 mm or 0.25 in.(see 6.1 for safety precautions).11.1.1.1 When puncturing the packaging to a
29、llow injection of the dye penetrant solution, care should be taken not to puncturethrough or damage other package surfaces. Puncturing of the package is facilitated if it is done adjacent to a dummy device insidethe package. The device will provide a tenting effect that will separate the two sides o
30、f the package, reducing the chance ofaccidental puncture of both sides.11.1.2 Visually examine the seal area through the transparent side of the package. Observe the package seal area for penetrationof the dye solution across the seal width. Channels in the seal will be readily detected. Use 5 secon
31、ds per side max as a guide fora 4 sided package. Total time should be less than or equal to 20 seconds. With prolonged exposure wicking of dye through theporous packaging will color the entire seal making defect detection difficult. An optical device with 5 to 20 magnification maybe used for detaile
32、d examination.11.1.3 Rotate the package as necessary to expose each seal edge to the dye penetrant solution. Inject additional dye as neededto insure complete edge exposure.11.2 Method B (Edge Dip Method):11.2.1 Select a container whose length is long enough to accommodate the longest sealed edge of
33、 the package.11.2.2 Pour enough dye into the container to cover the entire bottom surface to a minimum depth of approximately 36 mmor 0.1250.25 in.11.2.2.1 If the package being tested has excessive material beyond the seal, such as a chevron style opening feature, amodification must be made to the p
34、ackage. With a cutting instrument, remove the excessive material along the outside edge of thechevron seal to a distance of approximately 3 mm or 0.125 in. from the seal, taking care not to cut into the seal area. Removalof the excess material will allow the dye solution to come into close proximity
35、 to the seal.11.2.3 Lower one of the edges of the package into the dye solution so that it briefly touches the dye along the entire edge ofthe seal. This needs to be a brief dip process, just long enough to completely wet the edge.11.2.4 Remove the package in its dipped orientation, and verify that
36、the entire seal edge has been exposed to the dye solution.Observe the package seal area, through the transparent side, for penetration of the dye solution across the seal width. Use 5 secondsper side max as a guide for a 4 sided package. Total time should be less than or equal to 20 seconds.11.2.5 A
37、n optical device with 5 to 20 magnification may be 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 area beyond the outer edge of the seal.11.3.1 Pour dye solution into an open co
38、ntainer.11.3.2 Using a finger or the end of a paper clip, carefully push back the extended edge of the porous material away from thetransparent material.11.3.3 Insert eyedropper or pipette into the dye solution.11.3.4 With the transparent side of the package facing the operator, lay a bead of the dy
39、e solution along the top edge of thepackage 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, while applying solution until the entire package seal is exposed to thesolution. Otherwise, apply sol
40、ution to one side of the package at a time.11.3.6 Observe the package seal area for penetration of the dye solution across the seal width. Use 5 seconds per side max asa guide for a 4 sided package. Total time should be less than or equal to 20 seconds.12. Report12.1 Report the following information
41、: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.12.1.4 Identification of the
42、 dye penetrant solution if different 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 of the seal or to the interior of the seal via a defined channel shall betaken as an indication of the
43、 presence of a leakage site.12.1.6.2 Evidence of dye penetration through the porous material through general wetting of the surface (wicking) shall not betaken as an indication of the presence of a leakage site.12.1.6.3 A qualitative description or sketch of the leakage sites.F1929 15312.1.6.4 Any d
44、eviation from standard.13. Precision and Bias13.1 Injection Method:13.1.1 Between June 1997, and March 1998 test packages from four manufacturers were examined using this method by threeindependent laboratories. Defects were intentionally created in the package seals by placing wires of 50 m (0.002
45、in.) diameterin the seal area. When the wires were removed, a channel approximately the size of the wire was created in the seal. For eachspecimen set, 50 packages were produced, 25 with wire created defects and 25 controls with no artificial defects. The results areshown in Table 1 as (the number o
46、f correctly identified defects)/ (the number of test packages).13.1.2 The results show that when using the dye penetrant on packages with one side consisting of a porous breathablemembrane, there is more than 95 % confidence that channels in package seals will be detected if they are equivalent in s
47、ize in thosemade with a 50 m (0.002 in.) wire. In this test series, significant reductions in test performance (probability of detecting a defect60 %) were observed with pouches fabricated with film on both surfaces and with indicator dyes other than toluidine blue.Previous testing had shown signifi
48、cantly poorer detection with other wetting agents. These test results are therefore specific for thisdye and wetting agent formulation.13.1.3 The above P the details are given in RR:F02-1032.513.2.2 When combining the edge dip data population of all labs, the results show that this method provides t
49、he correct responseof detecting channels created by a 50 m wire in seals 95 % of the time. The 95 % confidence interval is 93.8 % to 96.0 %. Theresults of correctly identified, false positives and false negatives are shown in Tables 2-4.5 Supporting data have been filed at ASTM International Headquarters and may be obtained by requesting Research Report RR:F02-1032. Contact ASTM CustomerService at serviceastm.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# paperWi
