1、Designation: F3039 13Standard Test Method forDetecting Leaks in Nonporous Packaging or Flexible BarrierMaterials by Dye Penetration1This standard is issued under the fixed designation F3039; 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 () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method defines a procedure that will detect andlocate a leak equal to or greater than a
3、channel formed by a 50m 0.002 in. wire in the edge seals of a nonporous package.A dye penetrant solution is applied locally to the seal edge tobe tested for leaks. After contact with the dye penetrant for aminimum specified time, the package is visually inspected fordye penetration or, preferably, t
4、he seal edge is placed against anabsorbent surface and the surface inspected for staining fromthe dye.1.2 This test method is used for both transparent and opaquenonporous surfaces.1.3 This test method requires that the dye penetrant havegood contrast to the materials being tested and/or the absorbe
5、ntsurface.1.4 The values stated in either SI units or inch-pound unitsare to be regarded separately as standard. The values stated ineach system may not be exact equivalents; therefore, eachsystem shall be used independently of the other. Combiningvalues from the two systems may result in non-confor
6、mancewith the standard.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 applica-bility of regulatory limitations prior
7、 to use.2. Referenced Documents2.1 ASTM Standards:2E171 Practice for Conditioning and Testing Flexible BarrierPackaging2.2 ANSI Standards:3Z1.4 Sampling Procedures and Tables for Inspection byAttributes3. Terminology3.1 Definitions:3.1.1 dye penetrantan aqueous solution of a dye and asurfactant desi
8、gned to penetrate and indicate a defect.4. Significance and Use4.1 Contaminants may enter the package through leaks.Alternatively, product may be lost from the package throughleaks. These leaks are frequently found at seals betweenpackage components of the same or dissimilar materials.4.2 Ingress or
9、 egress of gas or moisture through leaks in apackage can also degrade sensitive contents.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 detect leakage,components that exhibit any ind
10、ication of leakage may berejected.4.4 These procedures are suitable for use to verify andlocate leakage sites. They are not quantitative. No indication ofleak size can be inferred from the test. Therefore, this methodis employed as a go/no-go test.4.5 This test is destructive. All package or compone
11、nt testsamples exposed to dye penetration testing may not be used forfinal product packaging.5. Apparatus5.1 Means of breaching one of the packaging materials suchas a small knife.5.2 Dye Dispenser, such as an eyedropper or syringe forinjection of the dye penetrant solution.5.3 Microscope or optical
12、 loop with magnification of 5 to20 (optional).1This test method is under the jurisdiction ofASTM Committee F02 on FlexibleBarrier Packaging and is the direct responsibility of Subcommittee F02.40 onPackage Integrity.Current edition approved Nov. 15, 2013. Published December 2013. DOI:10.1520/F3039-1
13、3.2For 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 onthe ASTM website.3Available from American National Standards Institute (ANSI
14、), 25 W. 43rd St.,4th Floor, New York, NY 10036, http:/www.ansi.org.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States15.4 Absorbent Surface, such as a white chromatographypaper, white filter paper, or white paper towels.5.5 Aqueous dye
15、penetrant solution consisting of a carrier,wetting agent, and indicator dye with a surface tension of 25dynes/cm or less. One possible dye penetrant solution formu-lation consists of, by weight:Wetting agent Polyethylene glycol octylphenyl etherA3%Indicator dye Toluidine blueB0.05 %Carrier Distilled
16、 water 96.95 %APolyethylene glycol octylphenyl ether is sold under the brand name Triton X-100.BThe chemical name for Toluidine blue is 3-Amino-7-(dimethylamino)-2-methylphenothiazin-5-ium chloride.5.5.1 Because of the viscosity of the polyethylene glycoloctylphenyl ether, the preparation of the sol
17、ution is most easilyaccomplished by first taring a container with about 10 % of therequired amount of distilled water on a scale. The appropriateamount of polyethylene glycol octylphenyl ether is added tothe distilled water by weight and the mixture stirred or shaken.Once the polyethylene glycol oct
18、ylphenyl ether is dissolved,the remaining distilled water can then be added, followed bythe toluidine blue dye.5.5.2 The solution must remain homogeneous. If precipitateis noted, the solution must be replaced.5.5.3 If substitutes for the toluidine blue and/or TritonX-100 are used, their precision an
19、d bias must be experimen-tally determined.6. Safety Precautions6.1 Injecting dye penetrant into a package with a hypoder-mic needle and syringe is a common method for performing theseal channel detection portion of this test. Caution should betaken if this practice is chosen as it can result in punc
20、ture of theskin with a contaminated needle. An alternative approach is todispense the dye penetrant via a flexible tube attached to asyringe through an opening formed with an appropriate cuttinginstrument.7. Test Specimen7.1 The test specimen may consist of a complete packagedproduct (blemished, rej
21、ected, or dummy devices may be usedif they will not affect test results and are recorded prior to thetest) to assess the package for channels in seals. Emptypackages, or edge seal samples may also be used for testing forchannels or leaks in the seals.8. Calibration and Standardization8.1 Because thi
22、s test is not quantitative, calibration is notapplicable.9. Sampling9.1 The number of samples tested should be adequate to bepredictive of performance. Caution should be taken wheneliminating samples with defects as this can bias results. SeeANSI ASQC Z1.4.10. Conditioning10.1 Packaging must be free
23、 of condensation or any othersource of liquid water. Water already in the channel, hole, orpotential leak point may render them undetectable with a dyepenetrant. If there is any indication that the package has beenexposed to any liquid, it must be thoroughly dried at its typicalstorage temperature b
24、efore testing.10.2 See Practice E171 for conditioning guidance.11. Procedure11.1 Testing for channels or leaks in the seal:11.1.1 Inject dye penetrant into the package or along sealedge at a volume of at least 0.25 ml per 25 mm 1 in. of seallength.NOTE 1If puncturing the packaging to allow injection
25、 of the dyepenetrant solution, care should be taken not to puncture through ordamage other package surfaces. Puncturing of the package is facilitated ifit is done adjacent to a dummy product inside the package. The productwill provide a tenting effect that will separate the two sides of the package,
26、reducing the chance of accidental puncture of both sides.11.1.2 Allow the dye penetrant solution to remain in contactwith the seal edge for approximately 5 s. Channels will bedetected within this time period.11.1.3 If the package has a transparent side, the seal may beexamined visually through this
27、side. An optical device with 5to 20 magnification may be used for detailed examination. Ifthe package is opaque or if additional verification is desired,the outside edge of the seal being tested should be placedagainst an absorbent surface for approximately 5 s. Aftercarefully lifting the package, e
28、xamine the absorbent surface.The presence of stains indicates a channel or leak.NOTE 2If the package being tested has unsealed material between theouter edge of the seal and the outer edge of the package (i.e., a “skirt”),fold back the skirt material when placing the edge seal against theabsorbent s
29、urface.11.1.4 Rotate the package as necessary to expose each sealedge to the dye penetrant solution and repeat the examinationdetailed in 11.1.2 and 11.1.3. Inject additional dye as needed toensure complete edge exposure.12. Report12.1 Report the following information:12.1.1 Lot number and source of
30、 material, date, time,location, and operator of test and complete identification ofmaterials being tested.12.1.2 Any conditioning of the materials.12.1.3 Dye penetrant formulation.12.1.4 Method of visual inspection: aided or unaided.12.1.5 Results:12.1.5.1 Evidence of dye penetration to the opposite
31、 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.12.1.5.2 Evidence of dye penetration to the absorbent sur-face shall be taken as the indication of the presence of aleakage site.12.1.5.3 A qualitative description
32、or sketch of the leakagesites.12.1.6 Any and all deviations from standard.F3039 13213. Precision and Bias13.1 The precision of this test method is based on aninter-laboratory study of ASTM WK21528, New Test Methodfor Detecting Leaks in Nonporous Packaging or FlexibleBarrier Materials by Dye Penetrat
33、ion, conducted in 2012. Tenlaboratories participated in this study. Channel defect sampleswere created with a 50 m (0.002 in.) Tungsten wire in a 9.5mm 0.375 in. wide seal. Note that none of the samples testedhad a skirt. Each group of 50 samples contained 2030randomly distributed defect samples, wi
34、th the balance of thesamples being defect-free. Each participant analyzed 200randomly coded samples (4 groups of 50 samples each). Everyanalyst reported results to indicate the presence or absence ofa channel. The results were summarized in Table 1 below; thedetails are given in RR:F02-1034.413.2 Bi
35、asThere is no bias for pass/fail test methods.13.3 The materials tested were identified as:13.3.1 Clear materials13.3.1.1 PET/LDPE13.3.1.2 OPP/sealant13.3.2 Opaque materials13.3.2.1 PET/Foil/LDPE13.3.2.2 PA/Foil/EAA14. Keywords14.1 channel; dye penetrant; flexible packaging; leaks; non-porousANNEX(M
36、andatory Information)A1. CAPILLARY ACTIONA1.1 The use of dye penetration to detect pinholes andchannels relies on capillary action. Capillary action is thetendency for liquids to spontaneously rise in small tubesagainst the force of gravity. It occurs when the adhesive forcesbetween the liquid and t
37、he surface of the walls of the tube isgreater than the cohesive forces between the liquid molecule.Capillary action explains why paper towels absorb liquids andwhy fluids are transported through plants.A1.2 A liquid will form an interface with a second liquid orgas. The actual physical chemistry of
38、such interface surfaces isextremely complex. Generally speaking, molecules within theliquid repel each other because of their close packing. Incontrast, molecules at the surface are less dense and attracteach other. Since these surface molecules only have otherliquid molecules on one side, the mecha
39、nical effect is that thesurface is in tension.5The resultant surface tension is measuredin dynes/cm and represented by the symbol . The surfacetension for water at 20 C 68 F is 73 dynes/cm.5Waterssurface tension can be altered dramatically with the addition ofcontaminants such as surfactants.A1.3 Wh
40、en a solid surface intersects with a liquid-gasinterface, the angle formed by the liquid is the contact angle .If the contact angle is less than 90, the liquid wets the solidand if it is greater than 90 it is nonwetting. The greater thedifference between the surface tension of the liquid and thesurf
41、ace energy of the solid surface, the more the liquid will wetthe surface of the solid and the smaller the contact angle .4Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:F02-1034. ContactASTM CustomerService at serviceastm.org.5W
42、hite, Frank M., Fluid Mechanics, McGraw-Hill, Inc. 1986.TABLE 1 Summary of ResultsTotalspecimenstestedFalsepositivesFalsenegatives95%confidenceintervalError rate(%)2000 2 4 99.1399.94 0.3FIG. A1.1F3039 133A1.4 The height to which the liquid will rise in a tube is afunction of both the surface tensio
43、n of the liquid and thecontact angle formed with the tubes surface. The relationship isrepresented by the equation6:h 52cosgr(A1.1)where: = liquid-air surface tension, = contact angle, = density of the liquid,g = acceleration due to gravity, andr = radius of the tube.A1.5 A pinhole or channel is in
44、essence a tube. Because thedye penetrant solution has a surface tension less than thesurface energy of the materials generally used for flexiblepackaging materials (see Table A1.1), it will readily wet thesurface of the pinhole or channel. The dye penetrant solutiondoes not need to be “pushed” into
45、the channel or hole. As longas the dye penetrant solution makes contact with the channel orhole, capillary action can occur.6Batchelor, G. K., An Introduction To Fluid Dynamics, Cambridge UniversityPress, 1967.FIG. A1.2TABLE A1.1 Surface Energy of Common Packaging Materials(untreated)AMaterialSurfac
46、e Free Energy(dynes/cm)Aluminum Foil 41.2Polyamide-6.6 (nylon 6,6) 44.3Polycaprolactum, aramid 6 (nylon 6) 45.4Polyethylene (PE) 33.5Polyethyleneterephthalate (PET) 44.0Polyisobutylene 33.2Polypropylene (PP) 30.2Polystyrene 40.7Polyvinyl acetate (PVA) 38.5Polyvinyl alcohol (PVOH) 44.2Polyvinyl chlor
47、ide (PVC) 40.1Polyvinylidene fluoride (Saran) 43.7Ahttp:/ 134ASTM 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 of any such p
48、atent 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 e
49、ither 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 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 copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohoc
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