ASTM F1929-23

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: F1929 − 23
Standard Test Method for
Detecting Seal Leaks in Porous Medical Packaging by Dye
Penetration
This standard is issued under the fixed designation F1929; 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 This test method defines materials and procedures that 2.1 ASTM Standards:
will detect and locate a leak equal to or greater than a channel F17 Terminology Relating to Primary Barrier Packaging
formed by a 50 μm (0.002 in.) wire in package edge seals 2.2 ANSI Standards:
formed between a transparent material and a porous sheet Z1.4 Sampling Procedures and Tables for Inspection by
material. A dye penetrant solution is applied locally to the seal Attributes
edge to be tested for leaks. After contact with the dye penetrant
3. Terminology
for a specified time, the package is visually inspected for dye
3.1 wicking—the migration of a liquid into the body of a
penetration.
fibrous material. This is distinct from a leak as defined in
1.2 Three dye application methods are covered in this test
Terminology F17.
method: injection, edge dip, and eyedropper.
3.2 dye penetrant—an aqueous solution of a dye and a
1.3 These test methods are intended for use on packages
surfactant designed to penetrate and indicate a defect location
with edge seals formed between a transparent material and a
in the time prior to the onset of wicking which could mask its
porous sheet material. The test methods are limited to porous
presence.
materials which can retain the dye penetrant solution and
3.3 channel—refer to definition in F17.
prevent it from discoloring the seal area for a minimum of 5
seconds. Uncoated papers are especially susceptible to leakage
4. Significance and Use
and must be evaluated carefully for use with each test method.
4.1 Harmful biological or particulate contaminants may
1.4 These test methods require that the dye penetrant
enter the medical package through leaks. These leaks are
solution have good contrast to the opaque packaging material.
frequently found at seals between package components of the
1.5 The values are stated in International System of Units
same or dissimilar materials. Leaks may also result from a
(SI units) and English units. Either is to be regarded as pinhole in the packaging material.
standard.
4.2 It is the objective of this test method to visually observe
1.6 This standard does not purport to address all of the
the presence of channel defects by the leakage of dye through
safety concerns, if any, associated with its use. It is the
them.
responsibility of the user of this standard to establish appro-
4.3 This dye penetrant procedure is applicable only to
priate safety, health, and environmental practices and deter-
individual leaks in a package seal. The presence of a number of
mine the applicability of regulatory limitations prior to use.
small leaks, as found in porous packaging material, which
1.7 This international standard was developed in accor-
could be detected by other techniques, will not be indicated.
dance with internationally recognized principles on standard-
4.4 There is no general agreement concerning the level of
ization established in the Decision on Principles for the
leakage that is likely to be deleterious to a particular package.
Development of International Standards, Guides and Recom-
However, since these tests are designed to detect leaks,
mendations issued by the World Trade Organization Technical
components that exhibit any indication of leakage are normally
Barriers to Trade (TBT) Committee.
rejected.
1 2
This test method is under the jurisdiction of ASTM Committee F02 on Primary For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Barrier Packagingand is the direct responsibility of Subcommittee F02.40 on contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Package Integrity. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved Nov. 15, 2023. Published December 2023. Originally the ASTM website.
approved in 1998. Last previous edition approved in 2015 as F1929 – 15. DOI: Available from American National Standards Institute (ANSI), 25 W. 43rd St.,
10.1520/F1929-23. 4th Floor, New York, NY 10036.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
F1929 − 23
4.5 These procedures are suitable to verify and locate is dispensed using a flexible tube attached to a syringe through
leakage sites. They are not quantitative. No indication of leak an opening formed with an appropriate cutting instrument.
size can be inferred from these tests. The methods are usually
7. Test Specimen
employed as a pass/fail test.
7.1 The test specimen shall consist of a complete packaged
4.6 The dye solution will wick through any porous material
device, empty packages, or edge seal samples. Blemished,
over time, but usually not within the maximum time suggested.
rejected or dummy products may be used if they will not affect
If wicking does occur, it may be verified by observing the
test results and are recorded prior to the test.
porous side of the subject seal area. The dye will have
discolored the surface of the material. Refer to Appendix X1
8. Calibration and Standardization
for details on wicking and guidance on the observance of false
8.1 Since these procedures are not quantitative, no calibra-
positives.
tion is required.
5. Apparatus
9. Sampling
5.1 Means of breaching one of the packaging materials such
9.1 The number of samples tested should be adequate to be
as a small knife. (Method A)
predictive of performance. Caution should be taken when
5.2 Dye Dispenser, such as an eyedropper or syringe for eliminating samples with defects as this can bias the results.
injection of the dye penetrant solution. (Method A)
See ANSI ASQC Z1.4.
5.3 Dye Solution Container. (Method B)
10. Conditioning
5.4 Scissors or other cutting instrument. (Method B)
10.1 Packaging must be free of condensation or any other
5.5 Eyedropper or 1 Mil. Pipette. (Method C) source of liquid water. Water already in the seal defects may
render them undetectable with a dye penetrant. If there is any
5.6 Microscope or optical loop with magnification of 5× to
indication that the package has been exposed to any liquid, it
20× (optional for all methods).
must be thoroughly dried at its typical storage temperature
5.7 Aqueous dye penetrant solution consisting of a carrier, a
before testing.
surfactant, and an indicator dye. The surfactant should be
10.2 If conditioning is required standard conditioning atmo-
nonionic. The chemical properties of the surfactant should be
sphere of 23 6 2°C or 73.4 6 3.6°F and 50 6 2 % relative
as follows: surface tension between 30 mN ⁄m to 33 mN ⁄m,
humidity is recommended, for a minimum of 24 hr. prior to
hydrophilic ⁄lipophilic balance (HLB) greater than 10, and
testing.
critical micelle concentration (cmc) less than 2000 ppm. The
formula of the solution by weight:
11. Procedure
Wetting agent/surfactant: 0.5 %
A 11.1 Method A (Injection Method):
Indicator dye: Toluidine blue 0.05 %
Carrier: Water 99.45 % 11.1.1 Inject sufficient dye penetrant into the package to
cover the longest edge to a depth of approximately 5 mm or
A
The chemical name for Toluidine blue is 3-Amino-7-(dimethylamino)-2-
0.25 in. (see 6.1 for safety precautions).
methylphenothiazin-5-ium chloride.
11.1.1.1 When puncturing the packaging to allow injection
NOTE 1—The solution must remain homogeneous. If precipitate is
of the dye penetrant solution, care should be taken not to
noted, the solution must be replaced.
puncture through or damage other package surfaces. Punctur-
5.7.1 If other colored or fluorescent dyes are substituted for
ing of the package is facilitated if it is done adjacent to a
toluidine blue, their precision and bias must be experimentally
dummy device inside the package. The device will provide a
determined.
tenting effect that will separate the two sides of the package,
5.7.2 Because of the viscosity of many surfactants, the
reducing the chance of accidental puncture of both sides.
preparation of the solution is most easily accomplished by first
11.1.2 Visually examine the seal area through the transpar-
taring a container with about 10 % of the required amount of
ent side of the package. Observe the package seal area for
water on a scale. The appropriate amount of surfactant is added penetration of the dye solution across the seal width. Channels
to the water by weight and the mixture gently stirred. Vigorous
in the seal will be readily detected. Use 5 seconds per side max
stirring or shaking is not recommended, as it may cause as a guide for a 4 sided package. Total time should be less than
foaming that may be difficult to dissipate. Once the surfactant
or equal to 20 seconds. With prolonged exposure wicking of
is dissolved, the remaining water can then be added, followed dye through the porous packaging will color the entire seal
by the toluidine blue dye.
making defect detection difficult. An optical device with 5× to
20× magnification may be used for detailed examination.
6. Safety Precautions 11.1.3 Rotate the package as necessary to expose each seal
edge to the dye penetrant solution. Inject additional dye as
6.1 Injecting dye penetrant into a package with a hypoder-
needed to insure complete edge exposure.
mic needle and syringe is a common method for performing
this test. This practice can result in puncture of the skin with a 11.2 Method B (Edge Dip Method):
contaminated needle and is therefore not recommended. Be- 11.2.1 Select a container whose length is long enough to
cause of this hazard, it is recommended that the dye penetrant accommodate the longest sealed edge of the package.
F1929 − 23
11.2.2 Pour enough dye into the container to cover the entire 12.1.6.1 Evidence of dye penetration to the opposite side of
bottom surface to a minimum depth of approximately 3–6 mm the seal via a defined channel shall be taken as an indication of
or 0.125–0.25 in. the presence of a leakage site.
11.2.2.1 If the package being tested has excessive material 12.1.6.2 Evidence of dye penetration through the porous
material through general wetting of the surface (wicking) shall
beyond the seal, such as a chevron style opening feature, a
modification must be made to the package. With a cutting not be taken as an indication of the presence of a leakage site.
instrument, remove the excessive material along the outside 12.1.6.3 A qualitative description or sketch of the leakage
edge of the chevron seal to a distance of approximately 3 mm sites.
or 0.125 in. from the seal, taking care not to cut into the seal 12.1.6.4 Any deviation from standard.
area. Removal of the excess material will allow the dye
13. Precision and Bias
solution to come into close proximity to the seal.
11.2.3 Lower one of the edges of the package into the dye
13.1 Injection Method:
solution so that it briefly touches the dye along the entire edge 13.1.1 Between June 1997, and March 1998 test packages
of the seal. This needs to be a brief dip process, just long
from four manufacturers were examined using this method by
enough to completely wet the edge. three independent laboratories. Defects were intentionally
11.2.4 Remove the package in its dipped orientation, and
created in the package seals by placing wires of 50 μm (0.002
verify that the entire seal edge has been exposed to the dye in.) diameter in the seal area. When the wires were removed, a
solution. Observe the package seal area, through the transpar-
channel approximately the size of the wire was created in the
ent side, for penetration of the dye solution across the seal seal. For each specimen set, 50 packages were produced, 25
width. Use 5 seconds per side max as a guide for a 4 sided
with wire created defects and 25 controls with no artificial
package. Total time should be less than or equal to 20 seconds. defects. The results are shown in Table 1 as (the number of
11.2.5 An optical device with 5× to 20× magnification may
correctly identified defects)/ (the number of test packages).
be used for detailed examination. 13.1.2 The results show that when using the dye penetrant
11.2.6 Repeat edge dip for the remaining seals. on packages with one side consisting of a porous breathable
membrane, there is more than 95 % confidence that channels in
11.3 Method C (Eyedropper Method):
package seals will be detected if they are equivalent in size in
NOTE 2—This method requires the package to have an unsealed area
those made with a 50 μm (0.002 in.) wire. In this test series,
beyond the outer edge of the seal.
significant reductions in test performance (probability of de-
11.3.1 Pour dye solution into an open container. tecting a defect <60 %) were observed with pouches fabricated
11.3.2 Using a finger or the end of a paper clip, carefully with film on both surfaces and with indicator dyes other than
push back the extended edge of the porous material away from toluidine blue. Previous testing had shown significantly poorer
the transparent material. detection with other wetting agents. These test results are
11.3.3 Insert eyedropper or pipette into the dye solution. therefore specific for this dye and wetting agent formulation.
11.3.4 With the transparent side of the package facing the
operator, lay a bead of the dye solution along the top edge of
TABLE 1 Results on Testing Seals with Channels Generated
the package between the porous and transparent material.
Using 50 μm (0.002 in.) Wires
Ensure entire edge has been wetted with the dye solution.
Test Site 1 2 3
11.3.5 For small packages slowly rotate the package, while
Sample 1: Breathable pouch; coated 44# paper
applying solution until the entire package seal is exposed to the
With defect 25/25 24/25 22/24
solution. Otherwise, apply solution to one side of the package
No defect 24/24 24/24 25/25
at a time.
A
Sample 2: Tray with breathable lid; dot coated TYVEK
11.3.6 Observe the package seal area for penetration of the
dye solution across the seal width. Use 5 seconds per side max
With defect 25/25 25/25 24/25
as a guide for a 4 sided package. Total time should be less than
No defect 25/25 25/25 25/25
or equal to 20 seconds.
Sample 3: Breathable pouch; coated TYVEK
12. Report
Wi
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