ASTM F2338-09(2020)
(Test Method)Standard Test Method for Nondestructive Detection of Leaks in Packages by Vacuum Decay Method
Standard Test Method for Nondestructive Detection of Leaks in Packages by Vacuum Decay Method
SIGNIFICANCE AND USE
5.1 Leaks in medical device, pharmaceutical, and food packages may result in the ingress of unwanted gases (most commonly oxygen), harmful microbiological, or particulate contaminants. Package leaks may appear as imperfections in the package components themselves or at the seal juncture between mated components. The ability to detect leaks is necessary to ensure consistency and integrity of packages.
5.2 After initial set-up and calibration, individual test operation may be semi-automatic, automatic, or manual. The test method permits non-destructive detection of leaks not visibly detectable. The test method does not require the introduction of any extraneous materials or substances, such as dyes or gases. However, it is important to physically mask or block off any package porous barrier surface during the test to prevent rapid loss of chamber vacuum resulting primarily from gas migration through the porous surface. Leak detection is based solely on the ability to detect the change in pressure inside the test chamber resulting from gas or vapor egress from a package challenged with vacuum.
5.3 This test is a useful research tool for optimizing package sealing parameters and for comparatively evaluating various packages and materials. This test method is also applicable to production settings as it is rapid, non-invasive, and non-destructive, making it useful for either 100 % on-line testing or to perform tests on a statistical sampling from the production operation.
5.4 Leak test results that exceed the permissible limits for the vacuum decay test are indicated by audible or visual signal responses, or both.
SCOPE
1.1 Test Packages—Packages that can be nondestructively evaluated by this test method include:
1.1.1 Rigid and semi-rigid non-lidded trays.
1.1.2 Trays or cups sealed with porous barrier lidding material.
1.1.3 Rigid, nonporous packages.
1.1.4 Flexible, nonporous packages.
1.2 Leaks Detected—This test method detects package leaks by measuring the rise in pressure (vacuum loss) in an enclosed evacuated test chamber containing the test package. Vacuum loss results from leakage of test package headspace gases and/or volatilization of test package liquid contents located in or near the leak. When testing for leaks that may be partially or completely plugged with the package’s liquid contents, the test chamber is evacuated to a pressure below the liquid’s vaporization pressure. All methods require a test chamber to contain the test package and a leak detection system designed with one or more pressure transducers. Test method sensitivities cited below were determined using specific product-package systems selected for the precision and bias studies summarized in Table 1. Table 1 also lists other examples of relevant product-package systems that can be tested for leakage by vacuum decay.
1.2.1 Trays or Cups (Non-lidded) (Air Leakage)—Hole or crack defects in the wall of the tray/cup of at least 50 μm in diameter can be detected. Nonlidded trays were tested at a Target Vacuum of –4·E4 Pa (–400 mbar).
1.2.2 Trays Sealed with Porous Barrier Lidding Material (Headspace Gas Leakage)—Hole or crack defects in the wall of the tray/cup of at least 100 μm in diameter can be detected. Channel defects in the seal area (made using wires of 125 μm in diameter) can be detected. Severe seal bonding defects in both continuous adhesive and dot matrix adhesive package systems can be detected. Slightly incomplete dot matrix adhesive bonding defects can also be detected. All porous barrier lidding material packages were tested at a Target Vacuum of –4·E4 Pa (–400 mbar). The sensitivity of the test for porous lidded packages is approximately E-2 Pa·m3·s-1 using a calibrated volumetric airflow meter.
1.2.3 Rigid, Nonporous Packages (Headspace Gas Leakage)—Hole defects of at least 5 μm in diameter can be detected. Plastic bottles with screw caps were tested at a target vacuum...
General Information
Relations
Standards Content (Sample)
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: F2338 − 09 (Reapproved 2020)
Standard Test Method for
Nondestructive Detection of Leaks in Packages by Vacuum
Decay Method
This standard is issued under the fixed designation F2338; 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 adhesive bonding defects can also be detected. All porous
barrier lidding material packages were tested at a Target
1.1 Test Packages—Packages that can be nondestructively
Vacuumof–4·E4Pa(–400mbar).Thesensitivityofthetestfor
evaluated by this test method include:
3 -1
porous lidded packages is approximately E-2 Pa·m ·s using a
1.1.1 Rigid and semi-rigid non-lidded trays.
calibrated volumetric airflow meter.
1.1.2 Trays or cups sealed with porous barrier lidding
material. 1.2.3 Rigid, Nonporous Packages (Headspace Gas
1.1.3 Rigid, nonporous packages. Leakage)—Hole defects of at least 5 µm in diameter can be
1.1.4 Flexible, nonporous packages. detected. Plastic bottles with screw caps were tested at a target
vacuum of –5·E4 Pa (–500 mbar). Using a calibrated volumet-
1.2 Leaks Detected—This test method detects package leaks
ric airflow meter, the sensitivity of the test is approximately
by measuring the rise in pressure (vacuum loss) in an enclosed
3 -1
E-3.4 Pa·m ·s .Air-filled glass syringes were tested at a target
evacuated test chamber containing the test package. Vacuum
vacuum of –7.5·E4 Pa (+250 mbar absolute) and again at a
loss results from leakage of test package headspace gases
target vacuum of about +1 mbar absolute. The sensitivity of
and/or volatilization of test package liquid contents located in
3 -1
both tests is approximately E-4.1 Pa·m ·s using a calibrated
or near the leak.When testing for leaks that may be partially or
volumetric airflow meter.
completely plugged with the package’s liquid contents, the test
chamber is evacuated to a pressure below the liquid’s vapor-
1.2.4 Rigid, Nonporous Packages (Liquid Leakage)—Hole
ization pressure.All methods require a test chamber to contain defects of at least 5 µm in diameter can be detected. This
the test package and a leak detection system designed with one
detection limit was verified using a population of water-filled
or more pressure transducers. Test method sensitivities cited
glass syringes tested at a target vacuum of about +1 mbar
below were determined using specific product-package sys-
absolute.
tems selected for the precision and bias studies summarized in
1.2.5 Flexible, Nonporous Packages (Gas or Liquid
Table 1. Table 1 also lists other examples of relevant product-
Leakage)—Such packages may also be tested by the vacuum
package systems that can be tested for leakage by vacuum
decay method. Sensitivity data for flexible packages were not
decay.
included in the precision and bias studies, although the use of
1.2.1 Trays or Cups (Non-lidded) (Air Leakage)—Hole or
vacuum decay for testing such packages is well known.
crack defects in the wall of the tray/cup of at least 50 µm in
diameter can be detected. Nonlidded trays were tested at a 1.3 Test Results—Test results are qualitative (Accept/
Target Vacuum of –4·E4 Pa (–400 mbar). Reject). Acceptance criteria are established by comparing
1.2.2 Trays Sealed with Porous Barrier Lidding Material
quantitative baseline vacuum decay measurements obtained
(Headspace Gas Leakage)—Hole or crack defects in the wall
from control, non-leaking packages to measurements obtained
of the tray/cup of at least 100 µm in diameter can be detected.
usingleakingpackages,andtomeasurementsobtainedwiththe
Channel defects in the seal area (made using wires of 125 µm
introduction of simulated leaks using a calibrated gas flow
in diameter) can be detected. Severe seal bonding defects in
meter.
both continuous adhesive and dot matrix adhesive package
1.4 The values stated in SI units are to be regarded as
systems can be detected. Slightly incomplete dot matrix
standard. No other units of measurement are included in this
standard.
1 1.5 This standard does not purport to address all of the
This test method is under the jurisdiction ofASTM Committee F02 on Primary
Barrier Packaging and is the direct responsibility of Subcommittee F02.40 on
safety concerns, if any, associated with its use. It is the
Package Integrity.
responsibility of the user of this standard to establish appro-
Current edition approved Nov. 15, 2020. Published December 2020. Originally
priate safety, health, and environmental practices and deter-
approved in 2003. Last previous edition approved in 2013 as F2338 – 09 (2013).
DOI: 10.1520/F2338-09R20. mine the applicability of regulatory limitations prior to use.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
F2338 − 09 (2020)
TABLE 1 Summary of Vacuum Decay Leak Tests Applications for Various Product-Packages Systems
A B
Package Examples Package Content Examples ASTM P&B Data Tables Target Vacuum
GAS LEAK TEST
PACKAGE APPLICATIONS AND PRECISION & BIAS STUDIES
C
Porous barrier lidded trays Empty 3, 4, 5 –400 mbar
Solids (tablets, capsules, powders, devices)
C
Nonlidded trays or cups Empty 2 –400 mbar
C
Plastic screw capped bottles Solids (tablets, capsules, powders) 6 –500 mbar
Liquids (with significant gas headspace volume)
C
Glass syringes Solids (lyophilized powders) 7, 8 +250 mbar
A
ADDITIONAL GAS LEAK TEST PACKAGE APPLICATIONS
Lidded (nonporous) trays or cups containing solid materials (for example, powders, tablets, capsules, devices)
Glass or plastic vials closed with elastomeric closures containing solid materials (for example, powders)
Glass or plastic vials closed with elastomeric closures, containing liquid materials, but with significant gas headspace volume
Flexible packages (for example pouches or bags) containing solid materials (for example, powders, devices)
LIQUID LEAK TEST (with or without gas headspace)
PACKAGE APPLICATIONS AND PRECISION & BIAS STUDIES
C
Glass syringes Liquids 9, 10 +1 mbar
A
ADDITIONAL LIQUID LEAK TEST PACKAGE APPLICATIONS
Ophthalmic dropper tip bottles containing liquid materials
Glass or plastic ampoules containing liquid materials
Glass or plastic vials with elastomeric closures containing liquid materials
Lidded (nonporous trays or cups) containing liquid materials
Flexible packages such as pouches or bags containing liquid materials
A
Examples of package types relevant to the specified leak test method are listed. The list is not intended to be all inclusive.
B
Target vacuum expressed as a negative mbar reading (for example, –400 mbar) refers to the measured test chamber pressure (vacuum) relative to atmospheric pressure.
Target vacuum expressed as a positive mbar reading (for example, +1 mbar) refers to the absolute pressure reading in the test chamber.
C
Packages used for the referenced ASTM Precision and Bias (P&B) studies.
1.6 This international standard was developed in accor- 3.2.2 control, non-leaking packages, n—packages without
dance with internationally recognized principles on standard- defects and properly sealed or closed according to manufac-
ization established in the Decision on Principles for the turer’s specifications.
Development of International Standards, Guides and Recom-
3.2.3 flexible, nonporous packages, n—packages that sig-
mendations issued by the World Trade Organization Technical
nificantly deflect when under vacuum, and are constructed of
Barriers to Trade (TBT) Committee.
malleable, nonporous materials. Examples include pouches or
bags made of polymeric, foil, or laminate films.
2. Referenced Documents
3.2.4 gas leaks, n—leak paths that allow the flow of gas
2.1 ASTM Standards:
from the test package.
D996 Terminology of Packaging and Distribution Environ-
3.2.5 liquid leaks, n—leak paths partially or fully filled with
ments
liquid.
E691 Practice for Conducting an Interlaboratory Study to
3.2.6 rigid, nonporous packages, n—packages that do not
Determine the Precision of a Test Method
significantlydeflectundervacuumandareconstructedofsolid,
F17 Terminology Relating to Primary Barrier Packaging
nonporous materials. Examples include plastic bottles with
F1327 Terminology Relating to Barrier Materials for Medi-
screw-thread or snap-on closures, glass or plastic vials with
cal Packaging (Withdrawn 2007)
elastomeric closures, and glass or plastic syringes.
3. Terminology
3.2.7 semi-rigid trays or cups, n—trays made of material
that retain shape upon deflection. For example, thermoformed
3.1 Definitions—Fordefinitionsusedinthistestmethod,see
PETE or PETG trays are considered semi-rigid trays.
Terminologies D996, F17, and F1327.
3.2.8 spotty or mottled seals, n—an incomplete adhesive
3.2 Definitions of Terms Specific to This Standard:
bond made between a package tray or cup and porous lidding
3.2.1 baseline vacuum decay, n—the extent of vacuum
materialthatcanbevisiblyidentifiedbyadistinctivepatternof
change within the test chamber over time demonstrated by a
dots, spotting or mottling on the tray sealing surface after the
control, non-leaking package.
lid is removed.
3.2.9 volumetric airflow meter, n—a calibration tool that can
be used to provide an artificial leak of known volumetric
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
airflow rate into the test chamber for verification of instrument
Standards volume information, refer to the standard’s Document Summary page on
sensitivity. Airflow meters should be calibrated to NIST
the ASTM website.
standards.The operational range of the meter should reflect the
The last approved version of this historical standard is referenced on
www.astm.org. desired limit of sensitivity for the intended leak test.
F2338 − 09 (2020)
3.3 Definitions of Test Cycle and Critical Parameters 5. Significance and Use
Terms—For terms and abbreviations relating to the test cycle
5.1 Leaks in medical device, pharmaceutical, and food
and the critical parameters for establishing accept/reject limits,
packages may result in the ingress of unwanted gases (most
see Annex A1.
commonly oxygen), harmful microbiological, or particulate
contaminants. Package leaks may appear as imperfections in
4. Summary of Test Method
the package components themselves or at the seal juncture
between mated components. The ability to detect leaks is
4.1 The test package is placed in a test chamber to which
necessary to ensure consistency and integrity of packages.
vacuum is applied. The chamber is then isolated from the
vacuum source and a pressure transducer (absolute or gauge) 5.2 After initial set-up and calibration, individual test op-
eration may be semi-automatic, automatic, or manual. The test
alone or in combination with a second differential pressure
transducer, is used to monitor the test chamber for both the method permits non-destructive detection of leaks not visibly
detectable.Thetestmethoddoesnotrequiretheintroductionof
level of vacuum, as well as the change in vacuum over time.
any extraneous materials or substances, such as dyes or gases.
Vacuum decay, or rise in chamber pressure, is a result of
However, it is important to physically mask or block off any
packageheadspacegasbeingdrawnoutofthepackagethrough
package porous barrier surface during the test to prevent rapid
any leaks present, plus background noise. Vacuum decay can
lossofchambervacuumresultingprimarilyfromgasmigration
also result from the volatilization of packaged liquid that
through the porous surface. Leak detection is based solely on
partially or fully occludes the leak path. In this case, vacuum
the ability to detect the change in pressure inside the test
decay will only occur if the chamber test pressure is lowered
chamber resulting from gas or vapor egress from a package
below the liquid’s vaporization pressure.
challenged with vacuum.
4.2 Porous barrier lidded tray or cup packages are tested for
5.3 Thistestisausefulresearchtoolforoptimizingpackage
leaks located in the tray or cup, and at the lidding material/tray
sealing parameters and for comparatively evaluating various
seal junction. Leaks in the porous lidding material itself cannot
packages and materials. This test method is also applicable to
be detected. When testing such packages, steps are taken to
production settings as it is rapid, non-invasive, and non-
physically mask or block the porous barrier surface to prevent
destructive, making it useful for either 100 % on-line testing or
the migration of package gas through the porous lid. These
to perform tests on a statistical sampling from the production
steps may require some sample preparation, depending on the
operation.
masking approach required, but must be nondestructive and
5.4 Leak test results that exceed the permissible limits for
noninvasive. Vacuum decay from porous barrier lidded pack-
the vacuum decay test are indicated by audible or visual signal
ages may potentially include background noise from gas
responses, or both.
trapped between the lidding material and the masking surface,
or from transverse gas flow through the porous barrier material
6. Apparatus
itself at the lid/tray seal junction.
6.1 Vacuum Decay Leak Detection Apparatus—Thevacuum
4.3 The sensitivity of a test is a function of test package
decay leak apparatus includes a test chamber connected to a
design, transducer(s)’sensitivity, test chamber design, test sys-
vacuum decay test system and a volumetric airflow meter.
tem design, and critical test parameters of time and pressure.
6.2 Test Chamber—The test chamber has a lower compart-
The test system and leak test parameters selected for any given
ment (lower tooling) designed to nest the test package, and an
product-package system must be based on the package’s
upper lid (top tooling) for closing the test chamber. Fig. 1
contents (liquid or solid with significant or little gas
illustrates a test chamber designed for testing packages with
headspace), and the nature of the package (flexible or rigid,
porous barrier lidding material. The test fixture upper lid
porous or nonporous). Instruments with more sensitive pres-
consists of a flexible bladder to mask the package’s porous
suretransducersandwithminimalvoidvolumeswithinthetest
barrier during the test cycle. Figs. 2 and 3 illustrate test
chamber and the test system have the potential to detect the
chambers desig
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.