1、Designation: F3039 13F3039 15Standard 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 ca
2、se of revision, 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 Method A of this test method defines a procedure that will detect and locate a leak e
3、qual to or greater than a channelformed by a 50 m 0.002 in. wire in the edge seals of a nonporous package. A dye penetrant solution is applied locally to theseal edge to be tested for leaks.After contact with the dye penetrant for a minimum specified time, the package is visually inspectedfor dye pe
4、netration or, preferably, the seal edge is placed against an absorbent surface and the surface inspected for staining fromthe dye.1.2 Method B for this test method also defines a procedure that will detect and locate a leak equal to or greater than 10 m0.00039 in diameter in a nonporous flat sheet.
5、The flat sheet is placed on an absorbent surface and then a dye penetrant is spreadacross the surface of the sheet, preferably using a small roller to apply pressure on the sheet to ensure adequate contact betweenthe absorbent surface and the bottom surface of the sample being tested. The flat sheet
6、 is carefully removed and the absorbentsurface is inspected for staining from the dye.1.3 ThisThese test method ismethods are used for both transparent and opaque nonporous surfaces.1.4 ThisThese test method requiresmethods require that the dye penetrant have good contrast to the materials being tes
7、ted and/orthe absorbent surface.1.5 The values stated in either SI units or inch-pound units are to be regarded separately as standard. The values stated in eachsystem may not be exact equivalents; therefore, each system shall be used independently of the other. Combining values from thetwo systems
8、may result in non-conformance with the standard.1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regu
9、latorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2E171 Practice for Conditioning and Testing Flexible Barrier Packaging2.2 ANSI Standards:3Z1.4 Sampling Procedures and Tables for Inspection by Attributes3. Terminology3.1 Definitions:3.1.1 dye penetrantan aqueous solution of a
10、 dye and a surfactant designed 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 through leaks.These leaks are frequently found at seals between package components of the same or dissimi
11、lar materials.1 This test method is under the jurisdiction of ASTM Committee F02 on Flexible Barrier Packaging and is the direct responsibility of Subcommittee F02.40 on PackageIntegrity.Current edition approved Nov. 15, 2013Nov. 1, 2015. Published December 2013January 2015. Originally approved in 2
12、013. Last previous edition approved in 2013 asF303913. DOI: 10.1520/F3039-13.10.1520/F3039-15.2 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
13、Summary page on the ASTM website.3 Available from American National Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036, http:/www.ansi.org.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
14、 made to the previous version. Becauseit may not be technically possible to 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.
15、Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States14.2 Ingress or egress of gas or moisture through leaks in a package can also degrade sensitive contents.4.3 There is no general agreement concerning the level of leakage that is likely t
16、o be deleterious to a particular package.However, since these tests are designed to detect leakage, components that exhibit any indication of leakage may be rejected.4.4 These procedures are suitable for use to verify and locate leakage sites. They are not quantitative. No indication of leak sizecan
17、 be inferred from the test. Therefore, this method is employed as a go/no-go test.4.5 This test is destructive. AllThese tests are destructive. No package or component test samples exposed to dye penetrationtesting may not be used for final product packaging.5. Apparatus5.1 Means of breaching one of
18、 the packaging materials such as a small knife.5.2 Dye Dispenser, such as an eyedropper or syringe for injection of the dye penetrant solution.solution, or for application ofthe dye penetrant to the surface of the sheet sample for Method B.5.3 Microscope or optical loop with magnification of 5 to 20
19、 (optional).5.4 Absorbent Surface, such as a white chromatography paper, white filter paper, or white paper towels. Bright white printeror photocopier paper is preferred for the flat sheet (Method B) test.NOTE 1An embossed or uneven surface on the absorbent surface can inhibit consistent contact bet
20、ween the bottom surface of the sample and theabsorbent surface and can interfere with leak detection.5.5 Roller or other means to ensure intimate contact of the bottom of the sample being tested with the absorbent surface (MethodB only).5.6 Aqueous dye penetrant solution consisting of a carrier, wet
21、ting agent, and indicator dye with a surface tension of 2532dynes/cm or less. One possible dye penetrant solution formulation consists of, by weight:Wetting agent Polyethylene glycol octylphenyl etherA 3 %Indicator dye Toluidine blueB 0.05 %Carrier Distilled water 96.95 %A Polyethylene glycol octylp
22、henyl ether is sold under the brand name Triton X-100.B The chemical name for Toluidine blue is 3-Amino-7-(dimethylamino)-2-methylphenothiazin-5-ium chloride.5.6.1 Because of the viscosity of the polyethylene glycol octylphenyl ether, the preparation of the solution is most easilyaccomplished by fir
23、st taring a container with about 10 % of the required amount of distilled water on a scale. The appropriateamount of polyethylene glycol octylphenyl ether is added to the distilled water by weight and the mixture stirred or shaken. Oncethe polyethylene glycol octylphenyl ether is dissolved, the rema
24、ining distilled water can then be added, followed by the toluidineblue dye.5.6.2 The solution must remain homogeneous. If precipitate is noted, the solution must be replaced.5.6.3 If substitutes for the toluidine blue and/or Triton X-100 are used, their precision and bias must be experimentallydeter
25、mined.6. Safety Precautions6.1 Injecting dye penetrant into a package with a hypodermic needle and syringe is a common method for performing the sealchannel detection portion of this test. Caution should be taken if this practice is chosen as it can result in puncture of the skin witha contaminated
26、needle. An alternative approach is to dispense the dye penetrant via a flexible tube attached to a syringe throughan opening formed with an appropriate cutting instrument.7. Test Specimen7.1 The test specimen may consist of a complete packaged product (blemished, rejected, or dummy devices may be us
27、ed if theywill not affect test results and are recorded prior to the test) to assess the package for channels in seals. seals or leaks in the surfaceof the material. Empty packages, or edge seal samples or sheet material may also be used for testing for channels or leaks in theseals.seals or leaks i
28、n the surface of the material.8. Calibration and Standardization8.1 Because this test is not quantitative, calibration is not applicable.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 thi
29、s can bias results. See ANSI ASQC ANSI/ASQ Z1.4.F3039 15210. Conditioning10.1 Packaging must be free of condensation or any other source of liquid water. Water already in the channel, hole, or potentialleak point may render them undetectable with a dye penetrant. If there is any indication that the
30、package has been exposed to anyliquid, it must be thoroughly dried at its typical storage temperature before testing.10.2 See Practice E171 for conditioning guidance.11. Procedure11.1 Method ATesting for channels or leaks in the seal:11.1.1 Inject dye penetrant into the package or along seal edge at
31、 a volume of at least 0.25 ml per 25 mm 1 in. of seal length.NOTE 2If puncturing the packaging to allow injection of the dye penetrant solution, care should be taken not to puncture through or damage otherpackage surfaces. Puncturing of the package is facilitated if it is done adjacent to a dummy pr
32、oduct inside the package. The product will provide a tentingeffect that will separate the two sides of the package, reducing the chance of accidental puncture of both sides.11.1.2 Allow the dye penetrant solution to remain in contact with the seal edge for approximately 5 s. Channels will be detecte
33、dwithin this time period.11.1.3 If the package has a transparent side, the seal may be examined visually through this side. An optical device with 5 to20 magnification may be used for detailed examination. If the package is opaque or if additional verification is desired, the outsideedge of the seal
34、 being tested should be placed against an absorbent surface for approximately 5 s. After carefully lifting thepackage, examine the absorbent surface. The presence of stains indicates a channel or leak.NOTE 3If the package being tested has unsealed material between the outer edge of the seal and the
35、outer edge of the package (i.e., a “skirt”), foldback the skirt material when placing the edge seal against the absorbent surface.11.1.4 Rotate the package as necessary to expose each seal edge to the dye penetrant solution and repeat the examinationdetailed in 11.1.2 and 11.1.3. Inject additional d
36、ye as needed to ensure complete edge exposure.11.2 Method BTesting for holes or leaks in a flat surface:11.2.1 If testing a package, carefully cut the surface to be inspected so that the packaging material can lay flat.11.2.2 Place the sample, sheet or cut package, to be examined on an absorbent sur
37、face so that it lays flat without puckers orwrinkles. Analyst may use tape or small weights to secure the sheet sample to the adsorbent surface.11.2.3 Saturate an absorbent pad with dye penetrant solution and wipe across the surface of the test sample or apply dyepenetrant solution to the surface of
38、 the test sample with an eye dropper or pipette. Dye penetrant solution should contact all areasexhibiting questionable surface anomalies taking care not to allow dye penetrant solution to flow over the edge of the sample.11.2.4 Once areas of interest of the sample have been wiped with dye penetrant
39、 solution, use a small roller or other means toapply pressure to the sample to ensure adequate contact between the absorbent surface and the bottom surface of the sample beingtested. Wipe excess dye from sample using a clean absorbent pad and carefully lift the sample.11.2.5 Examine the absorbent su
40、rface circling any stains. The presence of stains indicates a hole or leak.12. Report12.1 Report the following information:12.1.1 Lot number and source of material, date, time, location, and operator of test and complete identification of materialsbeing tested.12.1.2 Any conditioning of the material
41、s.12.1.3 Dye penetrant formulation.12.1.4 Test(s) performed: Method A, Method B, or both.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 the
42、 indication of the presence of a leakage site.12.1.6.2 Evidence of dye penetration to the absorbent surface shall be taken as the indication of the presence of a leakage site.12.1.6.3 A qualitative description or sketch of the leakage sites.12.1.7 Any and all deviations from standard.13. Precision a
43、nd Bias13.1 Method AThe precision of this test method is based on an inter-laboratory study ofASTM WK21528, New Test Methodfor Detecting Leaks in Nonporous Packaging or Flexible Barrier Materials by Dye Penetration, interlaboratory study conductedin 2012. Ten laboratories participated in this study.
44、 Channel defect samples were created with a 50 m (0.002 in.) Tungsten wirein a 9.5 mm 0.375 in. wide seal. Note that none of the samples tested had a skirt. Each group of 50 samples contained 2030randomly distributed defect samples, with the balance of the samples being defect-free. Each participant
45、 analyzed 200 randomlyF3039 153coded samples (4 groups of 50 samples each). Every analyst reported results to indicate the presence or absence of a channel. Theresults were summarized in Table 1 below; ; the details are given in RR:F02-1034.413.1.1 The materials tested were identified as:13.1.1.1 Cl
46、ear materials.13.1.1.2 PET/LDPE13.1.1.3 OPP/sealant13.1.2 Opaque materials.13.1.2.1 PET/Al Foil/LDPE13.1.2.2 PA/Al Foil/EAATABLE 1 Summary of ResultsTotal specimenstestedFalsepositivesFalsenegatives95% confidenceintervalError rate(%)2000 2 4 99.1399.94 0.313.2 Method BThe precision of this test meth
47、od is based on an interlaboratory study conducted in 2013/2014. Eightlaboratories participated in this study. Pinhole defect samples were created by drilling holes in flat sheet materials with a laser. Eachgroup of 18 samples contained 3 control samples (no pinhole), and 3 samples each at 10 m, 20 m
48、, 30 m, 40 m, and 50 mrandomly distributed. Four sets of these samples were obtained, and the samples were returned to the study director after the firstfour labs tested them. The hole sizes of these samples were verified before they were sent out to the second set of four labs. Everyanalyst reporte
49、d results to indicate the presence or absence of a pinhole. The results were summarized in Table 2; the details aregiven in RR:F02-1040.513.2.1 The material used in the interlaboratory study for Method B was PET/Al Foil/PE.TABLE 2 Summary of Results A ,BHoleSize, mSampleSizeCorrectResponsesIncorrectResponsesProbabilityof DetectionCI LowerBoundCI Upperbound0 25 24 1 0.960 0.796 0.99910 26 20 6 0.769 0.564 0.91020 23 21 2 0.913 0.720 0.98930 23 22 1 0.957 0.781 0.99940 24 24 0 1.000 0.883 . . .50 23 23 0 1.000 0.878 . . .ASample size varies because s
