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ASTM D3078-02(2008)

(Test Method)

Standard Test Method for Determination of Leaks in Flexible Packaging by Bubble Emission

Standard Test Method for Determination of Leaks in Flexible Packaging by Bubble Emission

ABSTRACT
This test method covers the determination of gross leaks in flexible packaging containing a headspace gas by bubble emission. A vacuum chamber shall be any transparent container capable of withstanding approximately one atmosphere pressure differential, fitted with a vacuum-tight cover. A vacuum gage, an inlet tube from a source of vacuum, and an outlet tube to the atmosphere shall be connected to the chamber cover. Use an immersion fluid which does not degrade the package being tested. The test sample and test fluid shall be at equilibrium with normal room temperature. The procedures for testing are presented in details.
SCOPE
1.1 This test method covers the determination of gross leaks in flexible packaging containing a headspace gas. Test sensitivity is limited to 1 × 10−5 atm cm3/s (1 × 10−6 Pa m3/s) or even less sensitive as indicated in a recent interlaboratory test (reported in Section 12).
1.2 Small leaks may not be detected by this procedure. Viscoelastic effects on the products, or entrapped air, become significant and prevent passage through small openings. Positive pressure inside the pouch after the vacuum is drawn may force the product to plug small leaks. The size of the leak that can be detected is dependent upon the products contained, the nature of the packaging material, and the test parameters selected.
1.3 The values stated in inch-pound units are to be regarded as standard. The values given in parentheses are mathematical conversions to SI units that are provided for information only and are not considered standard.
1.4 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-Mar-2008
ICS
55.040 - Packaging materials and accessories
Technical Committee
F02 - Primary Barrier Packaging
Drafting Committee
F02.40 - Package Integrity
Current Stage
Ref Project

Relations

Replaces
ASTM D3078-02 - Standard Test Method for Determination of Leaks in Flexible Packaging by Bubble Emission
Effective Date
01-Apr-2008
Replaced By
ASTM D3078-02(2008)e1 - Standard Test Method for Determination of Leaks in Flexible Packaging by Bubble Emission
Effective Date
01-Apr-2008
Referred By
ASTM F2391-22 - Standard Test Method for Measuring Package and Seal Integrity Using Helium as the Tracer Gas
Effective Date
01-Apr-2008
Referred By
ASTM D6653/D6653M-13(2021) - Standard Test Methods for Determining the Effects of High Altitude on Packaging Systems by Vacuum Method
Effective Date
01-Apr-2008
Referred By
ASTM D4991-07(2023) - Standard Test Method for Leakage Testing of Empty Rigid Containers by Vacuum Method
Effective Date
01-Apr-2008
Referred By
ASTM F2097-20 - Standard Guide for Design and Evaluation of Primary Flexible Packaging for Medical Products
Effective Date
01-Apr-2008

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ASTM D3078-02(2008) - Standard Test Method for Determination of Leaks in Flexible Packaging by Bubble EmissionASTM D3078-02(2008) - Standard Test Method for Determination of Leaks in Flexible Packaging by Bubble Emission
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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:D3078–02 (Reapproved 2008)
Standard Test Method for
Determination of Leaks in Flexible Packaging by Bubble
1
Emission
This standard is issued under the fixed designation D3078; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope F98 Practices for Determining Hermeticity of Electron
3
Devices by a Bubble Test
1.1 Thistestmethodcoversthedeterminationofgrossleaks
in flexible packaging containing a headspace gas. Test sensi-
3. Terminology
−5 3 −6 3
tivity is limited to 1 310 atm cm /s (1 310 Pa m /s) or
3.1 Definition:
even less sensitive as indicated in a recent interlaboratory test
3.1.1 leak—any opening in a flexible package that, contrary
(reported in Section 12).
to intention, either allows the contents to escape or substances
1.2 Small leaks may not be detected by this procedure.
to enter.
Viscoelastic effects on the products, or entrapped air, become
significant and prevent passage through small openings. Posi-
4. Apparatus
tive pressure inside the pouch after the vacuum is drawn may
4.1 Vacuum Chamber—Any transparent container capable
force the product to plug small leaks. The size of the leak that
of withstanding approximately one atmosphere pressure differ-
can be detected is dependent upon the products contained, the
ential, fitted with a vacuum-tight cover. A vacuum gage, an
nature of the packaging material, and the test parameters
inlet tube from a source of vacuum, and an outlet tube to the
selected.
atmosphere shall be connected to the chamber cover. The inlet
1.3 The values stated in inch-pound units are to be regarded
and outlet tubes shall be equipped with hand valves.Attached
as standard. The values given in parentheses are mathematical
to the underside of the cover shall be a transparent plate that
conversions to SI units that are provided for information only
willcloselyapproximatetheinsidedimensionsofthecontainer
and are not considered standard.
and be such a distance from the top of the container that when
1.4 This standard does not purport to address all of the
it is two-thirds filled with fluid, the attached plate will be
safety concerns, if any, associated with its use. It is the
positioned 1 in. (25 mm) under the fluid.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
5. Materials
bility of regulatory limitations prior to use.
5.1 Immersion Fluids—Use an immersion fluid which does
notdegradethepackagebeingtested.Fluidswithalowsurface
2. Referenced Documents
tension are generally more sensitive. Examples include water,
2
2.1 ASTM Standards:
3 water treated with a wetting agent, denatured alcohol, and
E425 Definitions of Terms Related to Leak Testing
mineral oil. Other possible fluids are listed in Test Method
E515 Test Method for Leaks Using Bubble Emission Tech-
E515 and Practices F98.
niques
6. Sampling
1
6.1 The number of specimens used in the test sample may
ThistestmethodisunderthejurisdictionofASTMCommitteeF02onFlexible
Barrier Packaging and is the direct responsibility of Subcommittee F02.40 on
be varied according to the nature of the product, its cost, its
Package Integrity.
size, and whether the specimens are taken from a production
Current edition approved April 1, 2008. Published May 2008. Originally
line in a normal packaging operation, or are few in number, or
approved in 1972. Last previous edition approved in 2002 as D3078–02. DOI:
10.1520/D3078-02R08. are to be used only for purposes of comparative evaluation of
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
procedures or materials.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
7. Test Specimen
the ASTM website.
3
Withdrawn. 7.1 Flexible Package, with or without its intended contents.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
D3078–02 (2008)
8. Conditioning 11.1.4 Astatement of the number of specimens included in
the test and the number of failures, if any.
8.1 The test sample and test fluid shall be at equilibrium
11.1.5 Whenthetestisperformedtocheckcompliancewith
with normal room temperature.
requirements, a statement that the sample did or did not meet
9. Procedure
the requirement, and identification of the source for the
requirement.
9.1 Submerge the specimen in fluid contained in the
...

This document is not anASTM standard and is intended only to provide the user of anASTM 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:D3078–94 Designation:D3078–02 (Reapproved 2008)
Standard Test Method for
Determination of Leaks in Flexible Packaging by Bubble
1
Emission
This standard is issued under the fixed designation D3078; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope
1.1 This test method covers the determination of gross leaks in flexible packaging containing a headspace gas. Test sensitivity
−5 3 −6 3
islimitedto1 310 atmcm /s(1 310 Pam /s)./s)orevenlesssensitiveasindicatedinarecentinterlaboratorytest(reported
in Section 12).
1.2 Smallleaksmaynotbedetectedbythisprocedure.Viscoelasticeffectsontheproducts,orentrappedair,becomesignificant
and prevent passage through small openings. Positive pressure inside the pouch after the vacuum is drawn may force the product
toplugsmallleaks.Thesizeoftheleakthatcanbedetectedisdependentupontheproductscontained,thenatureofthepackaging
material, and the test parameters selected.
1.3
1.3 The values stated in inch-pound units are to be regarded as standard. The values given in parentheses are mathematical
conversions to SI units that are provided for information only and are not considered standard.
1.4 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:
2
E425Terminology Relating to Leak Testing
3
E425 Definitions of Terms Related to Leak Testing
E515 Test Method for Leaks Using Bubble Emission Techniques
0
F98 Practices for Determining Hermieticity of Electron Devices by a Bubble Test
3. Terminology
3.1 Definition:
3.1.1 leak—any opening in a flexible package that, contrary to intention, either allows the contents to escape or substances to
enter.
4.
5.Apparatus
5.1
4.1 Vacuum Chamber—Anytransparentcontainercapableofwithstandingapproximatelyoneatmospherepressuredifferential,
fittedwithavacuum-tightcover.Avacuumgage,aninlettubefromasourceofvacuum,andanoutlettubetotheatmosphereshall
be connected to the chamber cover. The inlet and outlet tubes shall be equipped with hand valves. Attached to the underside of
the cover shall be a transparent plate that will closely approximate the inside dimensions of the container and be such a distance
1
ThistestmethodisunderthejurisdictionofASTMCommitteeF-2onFlexibleBarrierMaterialsandisthedirectresponsibilityofSubcommitteeF02.30onTestMethods.
Current edition approved March 15, 1994. Published May 1994. Originally published as D3078–72. Last previous edition D3078–84.
1
This test method is under the jurisdiction ofASTM Committee F02 on Flexible Barrier Packaging and is the direct responsibility of Subcommittee F02.40 on Package
Integrity.
Current edition approved April 1, 2008. Published May 2008. Originally approved in 1972. Last previous edition approved in 2002 as D3078–02.
2
Discontinued; see 1990 Annual Book of ASTM Standards, Vol 03.03.
2
ForreferencedASTMstandards,visittheASTMwebsite,www.astm.org,orcontactASTMCustomerServiceatservice@astm.org.For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
3
Withdrawn.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
D3078–02 (2008)
from the top of the container that when it is two-thirds filled with fluid, the attached plate will be positioned 1 in. (25 mm) under
the fluid.
6.5. Materials
6.1
5.1 Immersion Fluids— Use an immersion fluid which does not degrade the package being tested. Fluids with a low surface
tension are generally more sensitive. Examples include water, water treated with a wetting agent, denatured alcohol, and mineral
oil. Other possible fluids are listed in Test Method E515 and Practices F98.
7.
6. Sampling
7.1The6.1 The number of specimens used in the test sample may be varied according to the nature of the product, its cost, its
size, and whether the specimens are taken from a production line in a normal packaging operation, or are few in number, or are
to be used on
...

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1.2 The values stated in inch-pound units are to be regarded as standard. The values given in parentheses are mathematical conversions to SI units that are provided for information only and are not considered standard.  
1.3 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.4 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.

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ASTM F1884-04(2023)(Test Method)
Standard Test Methods for Determining Residual Solvents in Packaging Materials

SIGNIFICANCE AND USE
5.1 This test method is intended to measure volatile organic compounds that are emitted from packaging materials under high-temperature conditions.  
5.2 This test method may be useful in assisting in the development and manufacture of packaging materials having minimal retained packaging ink/adhesive solvents.  
5.3 Modification of this procedure by utilizing appropriate qualitative GC detection devices such as a mass spectrometer in place of the flame ionization detector may provide identification of volatile organics of unknown identity.
SCOPE
1.1 This test method covers determination of the amount of residual solvents released from within a packaging material contained in a sealed vial under a given set of time and temperature conditions and is a recommended alternative for Test Method F151.  
1.2 This test method covers a procedure for quantitating volatile compounds whose identity has been established and which are retained in packaging materials.  
1.3 The analyst should determine the sensitivity and reproducibility of the method by carrying out appropriate studies on the solvents of interest. The analyst is referred to Practice E260 for guidance.  
1.4 For purposes of verifying the identity of or identifying unknown volatile compounds the analyst is encouraged to incorporate techniques such as gas chromatography/mass spectroscopy, gas chromatography/infrared spectroscopy or other suitable techniques in conjunction with this test method.  
1.5 Sensitivity of this test method in the determination of the concentration of a given retained solvent must be determined on a case by case basis due to the variation in the substrate/solvent interaction between different types of samples.  
1.6 This test method does not address the determination of total retained solvents in a packaging material. Techniques such as multiple headspace extraction can be employed to this end. The analyst is referred to the manual supplied with the GC-Autosampling system for guidance.  
1.7 The values stated in SI units are to be regarded as the standard.  
1.8 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.9 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.

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ASTM F119-82(2022)(Test Method)
Standard Test Method for Rate of Grease Penetration of Flexible Barrier Materials (Rapid Method)

SIGNIFICANCE AND USE
4.1 This test method is valuable in the development and selection of flexible barrier materials suited for use as grease barriers.  
4.2 The test is rapid in comparison with other methods because of the extremely small quantity of oil required for detection (about 6 μg). The actual time to failure is a multiple of the values obtained by this test method. When permeation is through an absorbent structure such as kraft paper coated with polyethylene, the failure times will be longer and variable, depending on the variation in porosity and thickness of the structure.
SCOPE
1.1 This test method provides standard conditions for determining the rate of grease penetration of flexible barrier materials. Pinholes, which can be measured by a separate test, will increase the rate of grease penetration as determined by this test method.  
1.2 The values stated in SI units are to be regarded as standard. The values given in parentheses are for information only.  
1.3 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.4 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.

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ASTM F2391-22(Test Method)
Standard Test Method for Measuring Package and Seal Integrity Using Helium as the Tracer Gas

SIGNIFICANCE AND USE
5.1 The vacuum, bubble test method, as described in Test Method D3078, and various other leak detection methods described elsewhere (Test Method D4991, Guide E432, Test Method E493, Test Method E498, Test Method E499, and Test Method E1603) have been successfully used widely in various industries and applications to determine that a given package is or is not a “leaker.” The sensitivity of any selected leak test method has to be considered to determine its applicability to a specific situation.  
5.2 The procedures presented in this test method allow the user to carry out package and seal integrity testing with sufficient sensitivity to quantify seals in the previously defined moderate to fine seal ranges.  
5.3 By employing seal-isolating leak testing fixtures, packages constructed of various materials can be tested in the full range of seal performance requirements. Design of these fixtures is beyond the scope of this method.  
5.4 These seal/package integrity test procedures can be utilized as:  
5.4.1 A design tool,  
5.4.2 For tooling qualification,  
5.4.3 Process setup,  
5.4.4 Process validation tool,  
5.4.5 Quality assurance monitoring, or  
5.4.6 Research and development.
SCOPE
1.1 This test method includes several procedures that can be used for the measurement of overall package and seal barrier performance of a variety of package types and package forms, as well as seal/closure types. The basic elements of this method include:  
1.1.1 Helium (employed as tracer gas),  
1.1.2 Helium leak detector (mass spectrometer), and  
1.1.3 Package/product-specific test fixtures.  
1.1.4 Most applications of helium leak detection are destructive, in that helium needs to be injected into the package after the package has been sealed. The injection site then needs to be sealed/patched externally, which often destroys its saleability. Alternatively, if helium can be incorporated into the headspace before sealing, the method can be non-destructive because all that needs to be accomplished is to simply detect for helium escaping the sealed package.  
1.2 Two procedures are described; however the supporting data in Section 14 only reflects Procedure B (Vacuum Mode). The alternative, Sniffer Mode, has proven to be a valuable procedure for many applications, but may have more variability due to exactly the manner that the operator conducts the test such as whether the package is squeezed, effect of multiple small leaks compared to fewer large leaks, background helium concentration, package permeability and speed at which the scan is conducted. Further testing to quantify this procedure’s variability is anticipated, but not included in this version.  
1.2.1 Procedure A: Sniffer Mode—the package is scanned externally for helium escaping into the atmosphere or fixture.  
1.2.2 Procedure B: Vacuum Mode—the helium containing package is placed in a closed fixture. After drawing a vacuum, helium escaping into the closed fixture (capture volume) is detected. Typically, the fixtures are custom made for the specific package under test.  
1.3 The sensitivity of the method can range from the detection of:  
1.3.1 Large leaks—10-2 Pa·m 3/s to 10-5 Pa·m3/s (10–1 cc/sec/atm to 10-4 cc/sec/atm).  
1.3.2 Moderate leaks—10-5 Pa·m 3/s to 10-7 Pa·m3/s (10-4 cc/sec/atm to 10-6 cc/sec/atm).  
1.3.3 Fine leaks—10-7 Pa·m 3/s to 10-9 Pa·m3/s (10-6 cc/sec/atm to 10-8 cc/sec/atm).  
1.3.4 Ultra-Fine leak—10-9 Pa·m 3/s to 10-11 Pa·m3/s (10-8 cc/sec/atm to 10-10 cc/sec/atm).
Note 1: Conversion from cc/sec/atm to Pa·m3/s is achieved by multiplying by 0.1.  
1.4 The terms large, moderate, fine and ultra-fine are relative terms only and do not imply the acceptability of any leak rate. The individual application dictates the level of integrity needed. For many packaging applications, only “large leaks” are considered unacceptable and the ability to detect smaller leaks is immaterial. All leak rates referred...

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