ASTM F3039-15

Standard Test Method for Detecting Leaks in Nonporous Packaging or Flexible Barrier Materials by Dye Penetration

SIGNIFICANCE AND USE
4.1 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 dissimilar materials.  
4.2 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 to 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 size can be inferred from the test. Therefore, this method is employed as a go/no-go test.  
4.5 These tests are destructive. No package or component test samples exposed to dye penetration testing may be used for final product packaging.
SCOPE
1.1 Method A of this test method defines a procedure that will detect and locate a leak equal to or greater than a channel formed by a 50 µm [0.002 in.] wire in the edge seals of a nonporous package. A dye penetrant solution is applied locally to the seal edge to be tested for leaks. After contact with the dye penetrant for a minimum specified time, the package is visually inspected for dye penetration or, preferably, the seal edge is placed against an absorbent surface and the surface inspected for staining from the 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 µm [0.00039 in] diameter in a nonporous flat sheet. The flat sheet is placed on an absorbent surface and then a dye penetrant is spread across the surface of the sheet, preferably using a small roller to apply pressure on the sheet to ensure adequate contact between the absorbent surface and the bottom surface of the sample being tested. The flat sheet is carefully removed and the absorbent surface is inspected for staining from the dye.  
1.3 These test methods are used for both transparent and opaque nonporous surfaces.  
1.4 These test methods require that the dye penetrant have good contrast to the materials being tested and/or the 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 each system may not be exact equivalents; therefore, each system shall be used independently of the other. Combining values from the two systems 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 responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

General Information

• Status: Historical
• Publication Date: 31-Oct-2015
• ICS: 55.040 - Packaging materials and accessories
• Technical Committee: F02 - Primary Barrier Packaging
• Drafting Committee: F02.40 - Package Integrity

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: F3039 − 15
Standard Test Method for
Detecting Leaks in Nonporous Packaging or Flexible Barrier
Materials by Dye Penetration
This standard is issued under the fixed designation F3039; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 2. Referenced Documents
1.1 Method A of this test method defines a procedure that
2.1 ASTM Standards:
will detect and locate a leak equal to or greater than a channel
E171 Practice for Conditioning and Testing Flexible Barrier
formed by a 50 µm [0.002 in.] wire in the edge seals of a
Packaging
nonporous package. A dye penetrant solution is applied locally
2.2 ANSI Standards:
to the seal edge to be tested for leaks. After contact with the
Z1.4 Sampling Procedures and Tables for Inspection by
dye penetrant for a minimum specified time, the package is
Attributes
visually inspected for dye penetration or, preferably, the seal
edge is placed against an absorbent surface and the surface
3. Terminology
inspected for staining from the dye.
3.1 Definitions:
1.2 Method B for this test method also defines a procedure
3.1.1 dye penetrant—an aqueous solution of a dye and a
that will detect and locate a leak equal to or greater than 10 µm
surfactant designed to penetrate and indicate a defect.
[0.00039 in] diameter in a nonporous flat sheet. The flat sheet
is placed on an absorbent surface and then a dye penetrant is
4. Significance and Use
spread across the surface of the sheet, preferably using a small
roller to apply pressure on the sheet to ensure adequate contact
4.1 Contaminants may enter the package through leaks.
between the absorbent surface and the bottom surface of the
Alternatively, product may be lost from the package through
sample being tested. The flat sheet is carefully removed and the
leaks. These leaks are frequently found at seals between
absorbent surface is inspected for staining from the dye.
package components of the same or dissimilar materials.
1.3 These test methods are used for both transparent and
4.2 Ingress or egress of gas or moisture through leaks in a
opaque nonporous surfaces.
package can also degrade sensitive contents.
1.4 These test methods require that the dye penetrant have
4.3 There is no general agreement concerning the level of
good contrast to the materials being tested and/or the absorbent
leakage that is likely to be deleterious to a particular package.
surface.
However, since these tests are designed to detect leakage,
1.5 The values stated in either SI units or inch-pound units components that exhibit any indication of leakage may be
are to be regarded separately as standard. The values stated in rejected.
each system may not be exact equivalents; therefore, each
4.4 These procedures are suitable for use to verify and
system shall be used independently of the other. Combining
locate leakage sites. They are not quantitative. No indication of
values from the two systems may result in non-conformance
leak size can be inferred from the test. Therefore, this method
with the standard.
is employed as a go/no-go test.
1.6 This standard does not purport to address all of the
4.5 These tests are destructive. No package or component
safety concerns, if any, associated with its use. It is the
test samples exposed to dye penetration testing may be used for
responsibility of the user of this standard to establish appro-
final product packaging.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
1 2
This test method is under the jurisdiction of ASTM Committee F02 on Flexible For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Barrier Packaging and is the direct responsibility of Subcommittee F02.40 on contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
Package Integrity. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved Nov. 1, 2015. Published January 2015. Originally the ASTM website.
approved in 2013. Last previous edition approved in 2013 as F3039–13. DOI: Available from American National Standards Institute (ANSI), 25 W. 43rd St.,
10.1520/F3039-15. 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 States
F3039 − 15
5. Apparatus test) to assess the package for channels in seals or leaks in the
surface of the material. Empty packages, or edge seal samples
5.1 Means of breaching one of the packaging materials such
or sheet material may also be used for testing for channels or
as a small knife.
leaks in the seals or leaks in the surface of the material.
5.2 Dye Dispenser, such as an eyedropper or syringe for
injection of the dye penetrant solution, or for application of the
8. Calibration and Standardization
dye penetrant to the surface of the sheet sample for Method B.
8.1 Because this test is not quantitative, calibration is not
5.3 Microscope or optical loop with magnification of 5× to
applicable.
20× (optional).
9. Sampling
5.4 Absorbent Surface, such as a white chromatography
paper, white filter paper, or white paper towels. Bright white
9.1 The number of samples tested should be adequate to be
printer or photocopier paper is preferred for the flat sheet
predictive of performance. Caution should be taken when
(Method B) test.
eliminating samples with defects as this can bias results. See
NOTE 1—An embossed or uneven surface on the absorbent surface can
ANSI/ASQ Z1.4.
inhibit consistent contact between the bottom surface of the sample and
the absorbent surface and can interfere with leak detection.
10. Conditioning
5.5 Roller or other means to ensure intimate contact of the
10.1 Packaging must be free of condensation or any other
bottom of the sample being tested with the absorbent surface
source of liquid water. Water already in the channel, hole, or
(Method B only).
potential leak point may render them undetectable with a dye
5.6 Aqueous dye penetrant solution consisting of a carrier,
penetrant. If there is any indication that the package has been
wetting agent, and indicator dye with a surface tension of 32
exposed to any liquid, it must be thoroughly dried at its typical
dynes/cm or less. One possible dye penetrant solution formu-
storage temperature before testing.
lation consists of, by weight:
10.2 See Practice E171 for conditioning guidance.
A
Wetting agent Polyethylene glycol octylphenyl ether 3 %
B
Indicator dye Toluidine blue 0.05 %
11. Procedure
Carrier Distilled water 96.95 %
A
Polyethylene glycol octylphenyl ether is sold under the brand name Triton X-100.
11.1 Method A—Testing for channels or leaks in the seal:
B
The chemical name for Toluidine blue is 3-Amino-7-(dimethylamino)-2-
11.1.1 Inject dye penetrant into the package or along seal
methylphenothiazin-5-ium chloride.
edge at a volume of at least 0.25 ml per 25 mm [1 in.] of seal
5.6.1 Because of the viscosity of the polyethylene glycol
length.
octylphenyl ether, the preparation of the solution is most easily
NOTE 2—If puncturing the packaging to allow injection of the dye
accomplished by first taring a container with about 10 % of the
penetrant solution, care should be taken not to puncture through or
required amount of distilled water on a scale. The appropriate
damage other package surfaces. Puncturing of the package is facilitated if
amount of polyethylene glycol octylphenyl ether is added to
it is done adjacent to a dummy product inside the package. The product
the distilled water by weight and the mixture stirred or shaken. will provide a tenting effect that will separate the two sides of the package,
reducing the chance of accidental puncture of both sides.
Once the polyethylene glycol octylphenyl ether is dissolved,
the remaining distilled water can then be added, followed by
11.1.2 Allow the dye penetrant solution to remain in contact
the toluidine blue dye.
with the seal edge for approximately 5 s. Channels will be
5.6.2 The solution must remain homogeneous. If precipitate
detected within this time period.
is noted, the solution must be replaced.
11.1.3 If the package has a transparent side, the seal may be
5.6.3 If substitutes for the toluidine blue and/or Triton
examined visually through this side. An optical device with 5×
X-100 are used, their precision and bias must be experimen-
to 20× magnification may be used for detailed examination. If
tally determined. the package is opaque or if additional verification is desired,
the outside edge of the seal being tested should be placed
6. Safety Precautions
against an absorbent surface for approximately 5 s. After
carefully lifting the package, examine the absorbent surface.
6.1 Injecting dye penetrant into a package with a hypoder-
The presence of stains indicates a channel or leak.
mic needle and syringe is a common method for performing the
seal channel detection portion of this test. Caution should be
NOTE 3—If the package being tested has unsealed material between the
taken if this practice is chosen as it can result in puncture of the outer 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 the
skin with a contaminated needle. An alternative approach is to
absorbent surface.
dispense the dye penetrant via a flexible tube attached to a
syringe through an opening formed with an appropriate cutting 11.1.4 Rotate the package as necessary to expose each seal
edge to the dye penetrant solution and repeat the examination
instrument.
detailed in 11.1.2 and 11.1.3. Inject additional dye as needed to
7. Test Specimen ensure complete edge exposure.
7.1 The test specim
...

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. Because
it 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 version
of the standard as published by ASTM is to be considered the official document.
Designation: F3039 − 13 F3039 − 15
Standard Test Method for
Detecting Leaks in Nonporous Packaging or Flexible Barrier
Materials by Dye Penetration
This standard is issued under the fixed designation F3039; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope
1.1 This Method A of this test method defines a procedure that will detect and locate a leak equal to or greater than a channel
formed by a 50 μm [0.002 in.] wire in the edge seals of a nonporous package. A dye penetrant solution is applied locally to the
seal edge to be tested for leaks. After contact with the dye penetrant for a minimum specified time, the package is visually inspected
for dye penetration or, preferably, the seal edge is placed against an absorbent surface and the surface inspected for staining from
the 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 μm
[0.00039 in] diameter in a nonporous flat sheet. The flat sheet is placed on an absorbent surface and then a dye penetrant is spread
across the surface of the sheet, preferably using a small roller to apply pressure on the sheet to ensure adequate contact between
the absorbent surface and the bottom surface of the sample being tested. The flat sheet is carefully removed and the absorbent
surface 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 tested and/or
the 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 each
system may not be exact equivalents; therefore, each system shall be used independently of the other. Combining values from the
two systems 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 responsibility
of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory
limitations prior to use.
2. Referenced Documents
2.1 ASTM Standards:
E171 Practice for Conditioning and Testing Flexible Barrier Packaging
2.2 ANSI Standards:
Z1.4 Sampling Procedures and Tables for Inspection by Attributes
3. Terminology
3.1 Definitions:
3.1.1 dye penetrant—an aqueous solution of a dye and a surfactant designed to penetrate and indicate a defect.
4. Significance and Use
4.1 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 dissimilar materials.
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 Package
Integrity.
Current edition approved Nov. 15, 2013Nov. 1, 2015. Published December 2013January 2015. Originally approved in 2013. Last previous edition approved in 2013 as
F3039–13. DOI: 10.1520/F3039-13.10.1520/F3039-15.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Available from American National Standards Institute (ANSI), 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 States
F3039 − 15
4.2 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 to 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 size
can 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 penetration
testing may not be used for final product packaging.
5. Apparatus
5.1 Means of breaching one of 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 of
the dye penetrant to the surface of the sheet sample for Method B.
5.3 Microscope or optical loop with magnification of 5× to 20× (optional).
5.4 Absorbent Surface, such as a white chromatography paper, white filter paper, or white paper towels. Bright white printer
or photocopier paper is preferred for the flat sheet (Method B) test.
NOTE 1—An embossed or uneven surface on the absorbent surface can inhibit consistent contact between the bottom surface of the sample and the
absorbent 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 (Method
B only).
5.6 Aqueous dye penetrant solution consisting of a carrier, wetting agent, and indicator dye with a surface tension of 2532
dynes/cm or less. One possible dye penetrant solution formulation consists of, by weight:
A
Wetting agent Polyethylene glycol octylphenyl ether 3 %
B
Indicator dye Toluidine blue 0.05 %
Carrier Distilled water 96.95 %
A
Polyethylene glycol octylphenyl 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 easily
accomplished by first taring a container with about 10 % of the required amount of distilled water on a scale. The appropriate
amount of polyethylene glycol octylphenyl ether is added to the distilled water by weight and the mixture stirred or shaken. Once
the polyethylene glycol octylphenyl ether is dissolved, the remaining distilled water can then be added, followed by the toluidine
blue 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 experimentally
determined.
6. Safety Precautions
6.1 Injecting dye penetrant into a package with a hypodermic needle and syringe is a common method for performing the seal
channel detection portion of this test. Caution should be taken if this practice is chosen as it can result in puncture of the skin with
a contaminated needle. An alternative approach is to dispense the dye penetrant via a flexible tube attached to a syringe through
an opening formed with an appropriate cutting instrument.
7. Test Specimen
7.1 The test specimen may consist of a complete packaged product (blemished, rejected, or dummy devices may be used if they
will not affect test results and are recorded prior to the test) to assess the package for channels in seals. seals or leaks in the surface
of the material. Empty packages, or edge seal samples or sheet material may also be used for testing for channels or leaks in the
seals.seals or leaks in the surface of the material.
8. Calibration and Standardization
8.1 Because this test is not quantitative, calibration is not applicable.
9. Sampling
9.1 The number of samples tested should be adequate to be predictive of performance. Caution should be taken when
eliminating samples with defects as this can bias results. See ANSI ASQC ANSI/ASQ Z1.4.
F3039 − 15
10. Conditioning
10.1 Packaging must be free of condensation or any other source of liquid water. Water already in the channel, hole, or potential
leak point may render them undetectable with a dye penetrant. If there is any indication that the package has been exposed to any
liquid, it must be thoroughly dried at its typical storage temperature before testing.
10.2 See Practice E171 for conditioning guidance.
11. Procedure
11.1 Method A—Testing for channels or leaks in the seal:
11.1.1 Inject dye penetrant into the package or along seal edge at a volume of at least 0.25 ml per 25 mm [1 in.] of seal length.
NOTE 2—If puncturing the packaging to allow injection of the dye penetrant solution, care should be taken not to puncture through or damage other
package surfaces. Puncturing of the package is facilitated if it is done adjacent to a dummy product inside the package. The product will provide a tenting
effect 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 detected
within 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× to
20× magnification may be used for detailed examination. If the package is opaque or if additional verification is desired, the outside
edge of the seal being tested should be placed against an absorbent surface for approximately 5 s. After carefully lifting the
package, examine the absorbent surface. The presence of stains indicates a channel or leak.
NOTE 3—If the package being tested has unsealed material between the outer 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 the absorbent surface.
11.1.4 Rotate the package as necessary to expose each seal edge to the dye pene
...