ASTM F2095-01
(Test Method)Standard Test Methods for Pressure Decay Leak Test for Nonporous Flexible Packages With and Without Restraining Plates
Standard Test Methods for Pressure Decay Leak Test for Nonporous Flexible Packages With and Without Restraining Plates
SCOPE
1.1 These test methods cover the measurement of leaks in nonporous film, foil, or laminate flexible pouches and foil-sealed trays, which may be empty or enclose solid product. If product is enclosed, seals or surfaces cannot be in contact with water, oils, or other liquid.
1.2 These test methods will detect leaks at a rate of 1 104 sccs (standard cubic centimetres per second) or greater, in flexible packages. The limitation of leak rate is dependent on package volume as tested.
1.3 The following test methods are included:
1.3.1 Test Method A-- Pressure Decay Leak Test for Nonporous Flexible Packages Without Restraining Plates
1.3.2 Test Method B-- Pressure Decay Leak Test for Nonporous Flexible Packages With Restraining Plates
1.4 These test methods are destructive in that they require entry into the package to supply an internal pressure of gas, typically air or nitrogen, although other gases may be used. The entry connection into the flexible package must be leak-tight.
1.5 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
Relations
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:F2095–01
Standard Test Methods for
Pressure Decay Leak Test for Nonporous Flexible Packages
With and Without Restraining Plates
This standard is issued under the fixed designation F2095; 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.
1. Scope F17 Terminology Relating to Flexible Barrier Materials
F1327 TerminologyRelatingtoBarrierMaterialsforMedi-
1.1 These test methods cover the measurement of leaks in
cal Packaging
nonporous film, foil, or laminate flexible pouches and foil-
2.2 Other Document:
sealed trays, which may be empty or enclose solid product. If
ANSI/AAMI/ISO 11607 Packaging for Terminally Steril-
product is enclosed, seals or surfaces cannot be in contact with
ized Medical Devices
water, oils, or other liquid.
−4
1.2 Thesetestmethodswilldetectleaksatarateof1 310
3. Terminology
sccs (standard cubic centimetres per second) or greater, in
3.1 Definitions of Terms Specific to This Standard:
flexible packages. The limitation of leak rate is dependent on
3.1.1 integrity—the unimpaired physical condition of the
package volume as tested.
package. This implies that there are no leaks in the seals or
1.3 The following test methods are included:
body materials.
1.3.1 Test Method A—Pressure Decay Leak Test for Non-
3.1.2 leak—See Terminology F1327.
porous Flexible Packages Without Restraining Plates
3.1.3 nonporous—types of materials that are not purposely
1.3.2 Test Method B—Pressure Decay Leak Test for Non-
designed to transfer gases through their matrix.
porous Flexible Packages With Restraining Plates
3.1.4 restraining plates—plates of rigid material, for ex-
1.4 These test methods are destructive in that they require
ample, aluminum, that are used to restrict the movement of the
entry into the package to supply an internal pressure of gas,
package during inflation.
typicallyairornitrogen,althoughothergasesmaybeused.The
3.1.5 seal—See TerminologyF17.
entry connection into the flexible package must be leak-tight.
3.1.6 standard cubic centimetre per second (sccs)—theflow
1.5 This standard does not purport to address all of the
rate of a gas (air) at standard conditions of 20°C (68°F) and
safety concerns, if any, associated with its use. It is the
14.7 psig (1 atmosphere or 760 mm Hg).
responsibility of the user of this standard to establish appro-
3.1.6.1 Discussion—Conditions may be varied depending
priate safety and health practices and determine the applica-
on the source of data.Always check the definition being used.
bility of regulatory limitations prior to use.
4. Summary of Test Method
2. Referenced Documents
2 4.1 Detection of leak paths in flexible packages that have
2.1 ASTM Standards:
3 nonporous material surfaces and seals can be accomplished by
D1898 Practice for Sampling of Plastics
pressurization of the package to a fixed pressure, shutting off
D4332 Practice for Conditioning Containers, Packages, or
the pressure and connecting a pressure transducer. Observed
Packaging Components for Testing
changes in pressure indicate the presence of leakage paths in
E177 Practice for Use of the Terms Precision and Bias in
the package seals or pinholes in the surfaces.This leak may be
ASTM Test Methods
represented in decay pressure units or calculated leak rate
E691 Practice for Conducting an Interlaboratory Study to
units. To accomplish this technique, a leak-tight measuring
Determine the Precision of a Test Method
path must be available between the package interior volume
and the pressure transducer (see Fig. 1).
4.2 Restraining plates may be used to limit the volume of
These test methods are under the jurisdiction of ASTM Committee F02 on
the pressurized package. Because the sensitivity of these test
Flexible Barrier Materials and are the direct responsibility of Subcommittee F02.40
on Package Integrity. methods is dependent in part on the internal volume of the
Current edition approved April 10, 2001. Published June 2001.
package, the effect of restraining plate use is to increase the
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
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. Available from American National Standards, Institute, 11 W. 42nd St., 13th
Withdrawn. Floor, New York, NY 10036.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
F2095–01
FIG. 1 Leak-Tight Entry System
sensitivity of the test (see Fig. 2). SeeAppendix X1 for further 5.3 The pressure decay method of leak testing is a physical
discussion of the effects of restraining plates on these test measure of package integrity.When testing medical packaging
methods.
which must conform to ISO 11607 standards, it may necessary
to verify the results of the pressure decay test method with
5. Significance and Use
other sterile package integrity test methods.
5.1 These test methods provide a rapid, simple to apply
5.4 Test Method A allows packages to be pressurized
method to detect small leaks in flexible package seals or walls
−4 without restraint. In Test Method A the pouch, tray, or other
at the leak rate level of greater than 1 3 10 sccs, thus
type package will contain a volume of air defined by its
providing a measure of package integrity.
mechanical configuration and its ability to resist internal
5.2 Whiletheoreticalleakratesensitivitycanbeestablished
pressure applied. This test method requires that the package
bycalculation,thetestmeasurementisinpressureunitsandthe
reachastablevolumeconfiguration(stopstretching)tomakea
measuringinstrumentmustbecalibrated,certified,andverified
measurement.
with these units.
FIG. 2 Restraining Fixture with Leak-Tight Entry System
F2095–01
NOTE 4—As seen in the combined gas laws, the pressure change is a
5.5 Test Method B allows the use of rigid restraining plates
functionoftemperature.Testpackagesandthetestmedium(air)shouldbe
against the walls of the package to limit its volume and
at similar temperatures.
stabilize the package volume.
9. Procedure
6. Apparatus
9.1 Test Method A—No Restraining Plates:
6.1 Test Method A:
9.1.1 Package Preparation—The package may be tested
6.1.1 A measuring instrument that provides the following:
with or without the product enclosed. To maximize sensitivity
6.1.1.1 A means to detect pressure changes with sufficient
of the test, the smallest internal volume of the package is
sensitivity to achieve theoretical leak rates in the package
desired.
specification;
9.1.2 Instrument Preparation (see Annex A1 for informa-
6.1.1.2 Automatic timer controls to pressurize the package
tion on determining appropriate test parameters):
to a preset pressure, hold the pressure for a set time, and
9.1.2.1 Select and set the test pressure.
provide a time period during which pressure change data can
9.1.2.2 Select and set the timers for charge (pressurization),
be taken;
settle (stabilization), and test (data taking period).
6.1.1.3 A means to set pressure;
9.1.2.3 Select and set pressure decay limits (if available).
6.1.1.4 A means of holding and displaying the pressure
9.1.3 Attach the inflation probe (supply and sensor) to the
change inside the package at the end of the test cycle;
instrument.
6.1.1.5 Ameans (optional) to set pressure decay limits for a
9.1.4 Attach the leak-tight entry device and inflation probe
test method and alert the operator if the limit is exceeded.
sensor to the package (see Fig. 1).
6.1.2 Ameanstoenterthepackageinaleaktightmannerso
9.1.5 Begin the test by activating the timer controls and
that an inflation pressure can be applied to the package and
valves to inflate, hold, and measure the test pressure inside the
changes in internal pressure can be sensed.
package.
NOTE 1—It is important to verify the leak integrity of the entry means
9.1.6 Observe the pressure decay at the end of the test time
sothatitdoesnotcontributetothepressurechangessensedduringtesting.
period, and note if the pressure decay limit has been exceeded.
6.2 Test Method B—Using Restraining Plates:
NOTE 5—Choice of times depends on package variables and leak rate
6.2.1 The measuring instrument shall have the characteris-
requirements. For example, small changes in initial test pressure may
tics described in 6.1.1.1-6.1.1.5.
occur from flexible package stretch, thus slightly increasing its volume
6.2.2 Parallel, rigid plates are required. An ability to adjust
(decreasing its pressure) or from fixture contact or the expanding gas
plate separation is desirable. The surface of the plates should
medium. Increased stabilization time will allow these effects to become
providelimitedporosityinordertopreventblockingofpinhole
stable before the test data period begins. Test times are selected based on
required leakage rates or pressure decay criteria along with the package
leaks in the walls (see Fig. 2).
volume. See Annex A1 for further discussion.
NOTE 2—Several techniques have been used to provide a means to
9.2 Test Method B—With Restraining Plates:
prevent blocking or lowering of the leak rate in package material walls in
contact with the plates. These techniques include the use of semi-porous
9.2.1 Package Preparation—The package may be tested
plastic, scoring of plate surfaces and use of screen-type materials.
with or without the product enclosed. To maximize sensitivity
of the test, the smallest internal volume of the package is
6.2.3 Ameanstoenterthepackageinaleak-tightmannerso
desired. To achieve the minimum volume, the smallest gap
that an inflation pressure can be applied to the package and
between restraining plates is advisable.
changes in internal pressure can be sensed.
9.2.2 Instrument Preparation (see Annex A1 for informa-
NOTE 3—It is important to verify the leak integrity of the entry means
tion on determining appropriate test parameters):
sothatitdoesnotcontributetothepressurechangessensedduringtesting.
9.2.2.1 Select and set the test pressure.
9.2.2.2 Select and set the timers for charge (pressurization),
7. Sampling
settle (stabilization), and test (data taking period).
7.1 The sample size is chosen to permit an adequate
9.2.2.3 Select and set pressure decay limits (if available).
determination of representative performance. Practice D1898
9.2.3 Attach the inflation probe (supply and sensor) to the
provides guidance to test specimen selection.
instrument.
7.2 Sample identification should be made prior to testing to
9.2.4 Attach the leak-tight entry device and inflation probe
allowtheoperatortorefertospecifictestsamples,ifnecessary.
sensor to the package (Fig. 1).
Record information such that test results and anomalies are
9.2.5 Enclose the package and probe in the restraining
identifiable back to the individual specimens.
fixture.
8. Conditioning
9.2.6 Begin the test by activating the timer controls and
valves to inflate, hold, and measure the test pressure inside the
8.1 Package samples should be conditioned to obtain the
package.
same temperature conditions as exist for the test apparatus.
9.2.7 Observe the pressure decay at the end of the test time
Since measured pressure change is also a function of tempera-
period and note if the pressure decay limit has been exceeded.
ture, then the samples must be at a stable temperature. Most
testing will occur at standard laboratory conditions of 23 6
NOTE 6—Choice of times depends on package variables and leak rate
2°C (73 6 4°F) and 50 6 5% relative humidity. Other
requirements. For example, small changes in initial test pressure may
conditions should be recorded at the time of the test. occur from flexible package stretch, thus slightly increasing its volume
F2095–01
(decreasing its pressure) or from fixture contact or the expanding gas
95 % Repeatability 95 % Reproducibility
medium. Increased stabilization time will allow these effects to become
Pressure Decay Limit (Within Limit (Between
Material Average, psig Laboratory) Laboratories)
stable before the test data period begins. Test times are selected based on
required leak rates or pressure decay criteria along with the package −4 −4 −4
Foil pouch 149.560 3 10 32.283 3 10 32.283 3 10
−4 −4 −4
volume. See Annex A1 for further discussion.
Film pouch 195.540 3 10 13.748 3 10 14.918 3 10
−4 −4 −4
Foil tray 64.900 3 10 19.629 3 10 26.095 3 10
10. Report (Test Methods A and B)
11.3 The standard deviations among test results are as
follows.Thesestandarddeviationsaremultipliedbyafactorof
10.1 Report the following information:
2.8 to yield the respective limits previously stated.
10.1.1 Method used.
Test Method A—No Restraining Plates
10.1.2 Packagetype,size,materials,andlotnumbersshould
Repeatability Standard Reproducibility Standard
be traceable.
Material Deviation Deviation
10.1.3 Whether the package was tested empty or filled with
−4 −4
Foil pouch 35.591 3 10 68.547 3 10
−4 −4
product.
Film pouch 19.418 3 10 23.989 3 10
−4 −4
Foil tray 7.758 3 10 9.815 3 10
10.1.4 The apparatus used and settings for test pressure,
Test Method B—With Restraining Plates
timers,anddecaylimits.Otheroptionalapparatussettingsmay
Repeatability Standard Reproducibility Standard
be recorded such as restraining plate gap.
Material Deviation Deviation
10.1.5 Date, time, location, and operator’s name.
−4 −4
Foil pouch 11.529 3 10 11.529 3 10
−4 −4
Film pouch 4.910 3 10 5.328 3 10
10.1.6 Conditioning parameters and environmental condi-
−4 −4
Foil tray 7.010 3 10 9.320 3 10
tions at the time of test (if applicable).
NOTE 7—The study of these test methods was designed to define the
10.1.7 Package test number and pressure decay if pressure
precision of the test methods in cases where a leak is present. The
decay limit was exceeded.
previously stated precision data is based on an assumed “leak” in each
packagesamplethroughafixedorificemeasuring12.7µm.Thiscalibrated
11. Precision and Bias
orifice was included in the internal tested volume of each package to
simulatea“pinhole”leak.Thisartificialleakwasprogrammedintothetest
11.1 This interlaboratory study was conducted to evaluate
designbecauseaconsistentactualleakofthissizecannotbemanufactured
the precision of the pressure decay test method of leak
into the package.
detection in identifying a known leak in various sealed,
11.4 Bias in the sense of a consistent difference in test
nonporous empty packages. Two variations of the test method
resultsfromanacceptedreferencevaluedoesnotexistbecause
were examine
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.