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ASTM D3985-95

(Test Method)

Standard Test Method for Oxygen Gas Transmission Rate Through Plastic Film and Sheeting Using a Coulometric Sensor

Standard Test Method for Oxygen Gas Transmission Rate Through Plastic Film and Sheeting Using a Coulometric Sensor

SCOPE
1.1 This test method covers a procedure for determination of the steady-state rate of transmission of oxygen gas through plastics in the form of film, sheeting, laminates, coextrusions, or plastic-coated papers or fabrics. It provides for the determination of ( ) oxygen gas transmission rate (O 2 GTR), ( ) the permeance of the film to oxygen gas (PO 2 ), and ( ) oxygen permeability coefficient (PO 2 ) in the case of homogeneous materials.
1.2 This standard does not purport to address all of the safety problems, 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-Dec-1994
ICS
55.040 - Packaging materials and accessories
Technical Committee
F02 - Primary Barrier Packaging
Drafting Committee
F02.30 - Mechanical Dispensers
Current Stage
Ref Project

Relations

Replaced By
ASTM D3985-02 - Standard Test Method for Oxygen Gas Transmission Rate Through Plastic Film and Sheeting Using a Coulometric Sensor
Effective Date
10-May-2001

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ASTM D3985-95 - Standard Test Method for Oxygen Gas Transmission Rate Through Plastic Film and Sheeting Using a Coulometric SensorASTM D3985-95 - Standard Test Method for Oxygen Gas Transmission Rate Through Plastic Film and Sheeting Using a Coulometric Sensor
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ASTM D3985-95 - Standard Test Method for Oxygen Gas Transmission Rate Through Plastic Film and Sheeting Using a Coulometric Sensor
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NOTICE: This standard has either been superseded and replaced by a new version or
withdrawn.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: D 3985 – 95
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Test Method for
Oxygen Gas Transmission Rate Through Plastic Film and
1
Sheeting Using a Coulometric Sensor
This standard is issued under the fixed designation D 3985; 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 (e) indicates an editorial change since the last revision or reapproval.
¯
1. Scope 3.1.3 oxygen permeability coeffıcient (PO )—the product of
2
the permeance and the thickness of film. The permeability is
1.1 This test method covers a procedure for determination
meaningful only for homogeneous materials, in which case it is
of the steady-state rate of transmission of oxygen gas through
a property characteristic of the bulk material. This quantity
plastics in the form of film, sheeting, laminates, coextrusions,
should not be used, unless the relationship between thickness
or plastic-coated papers or fabrics. It provides for the determi-
and permeance has been verified on tests using several different
nation of (1) oxygen gas transmission rate (O GTR), (2) the
2
thicknesses of the material. The SI unit of oxygen permeability
permeance of the film to oxygen gas (PO ), and (3) oxygen
2
is the mol/m·s·Pa. The test conditions (see 3.1.1) must be
¯
permeability coefficient PO ) in the case of homogeneous
2
stated.
materials.
1.2 This standard does not purport to address all of the
4. Summary of Test Method
safety problems, if any, associated with its use. It is the
4.1 The oxygen gas transmission rate is determined after the
responsibility of the user of this standard to establish appro-
sample has equilibrated in a dry test environment. In this
priate safety and health practices and determine the applica-
context, a“ dry” environment is considered to be one in which
bility of regulatory limitations prior to use.
the relative humidity is less than 1 %.
2. Referenced Documents
4.2 The specimen is mounted as a sealed semi-barrier
2.1 ASTM Standards: between two chambers at ambient atmospheric pressure. One
D 1434 Test Method for Determining Gas Permeability chamber is slowly purged by a stream of nitrogen and the other
2
Characteristics of Plastic Film and Sheeting
chamber contains oxygen. As oxygen gas permeates through
3
D 1898 Practice for Sampling of Plastics the film into the nitrogen carrier gas, it is transported to the
coulometric detector where it produces an electrical current,
3. Terminology
the magnitude of which is proportional to the amount of
3.1 Definitions: :
oxygen flowing into the detector per unit time.
3.1.1 oxygen transmission rate (O GTR)—the quantity of
2
oxygen gas passing through a unit area of the parallel surfaces 5. Significance and Use
of a plastic film per unit time under the conditions of test. The
5.1 The O GTR is an important determinant of the packag-
2
2
SI unit of transmission rate is the mol/(m ·s). The test condi-
ing protection afforded by barrier materials. It is not, however,
tions, including temperature and oxygen partial pressure on
the sole determinant, and additional tests, based on experience,
both sides of the film must be stated.
must be used to correlate packaging performance with O GTR.
2
3
3.1.1.1 A commonly used unit of O GTR is the cm (STP)/
2
It is suitable as a referee method of testing, provided that the
2 3
m ·d) at one atmosphere pressure difference where 1 cm (STP)
purchaser and the seller have agreed on sampling procedures,
is 44.62 μmol, 1 atm is 0.1013 MPa, and one day is
standardization procedures, test conditions, and acceptance
3
86.4 3 10 s. The O GTR in SI units is obtained by multiplying
2
criteria.
−10
the value in inch-pound units by 5.160 3 10 .
5.2 Limited statistical data on correlations with Test Method
4
3.1.2 oxygen permeance (PO )—the ratio of the O GTR to
2 2
D 1434 methods are available. However, the oxygen transmis-
the difference between the partial pressure of O on the two
2
sion rate of a standard reference material (see 12.1) as
2
sides of the film. The SI unit of permeance is the mol/(m ·s·Pa).
determined manometrically by the National Bureau of Stan-
The test conditions (see 5.1) must be stated.
dards, is in good agreement with the values obtained in the
coulometric interlaboratory test using material from the same
1
This test method is under the jurisdiction of ASTM Committee F-2 on Flexible
manufacturing lot. Thus, this test method may be used as a
Barrier Materials and is the direct responsibility of Subcommittee F02.30 on Test
referee method.
Methods.
Current edition approved Sept. 10, 1995. Publis
...

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5.1 This practice is valuable in determining the resistance of flexible packaging materials to flex-formed pinholes. Conditioning levels A, B, or C are typically used. Reference Practice E171 and Guide F2097.  
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5.3 This practice does not measure or condition materials for abrasion related to flex failure.  
5.4 Failures in the integrity of one or more of the plies of a multi-ply structure may require alternative testing. Supplementary permeation testing using gas or water vapor can be used in conjunction with the flex conditioning to measure the loss of ply integrity. Other test methods may be used after flexing for assessment of presence of pinholes. For a list of test methods, refer to Guide F2097.
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1.1 This practice covers conditioning of flexible barrier materials for the determination of flex resistance. Subsequent testing can be performed to determine the effects of flexing on material properties. These tests are beyond the scope of this practice.  
1.2 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.  
1.3 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.  
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5.1 Materials such as engineered thermoplastic films are often used for flexible barrier packaging. However, handling and transportation can cause abrasion to the packaging film and possibly compromise the integrity of the contents (for example, sterility of a medical device). This test method provides a comparative ranking of material performance that can be used as an indication of relative end-use performance.  
5.2 The resistance of material surfaces to abrasion, as measured on a testing machine under laboratory conditions, is only one of several factors contributing to wear performance or durability as experienced in the actual use of the material. While abrasion resistance and durability are frequently related, the relationship varies with different end uses and different factors may be necessary in any calculation of predicted durability from specific abrasion data.  
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5.4 This test method may not be suitable for all films, including the following cases:  
5.4.1 Films that stretch and generate a ripple in the abraded region during testing,  
5.4.2 Films that have a thickness greater than 0.25 mm (0.010 in.), or are of such rigidity that forming over the mandrel would cause internal stresses that weaken the film, and  
5.4.3 Conductive films.
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1.1 This test method covers the determination of the abrasion resistance of flexible non-conductive films and packaging materials using a weighted stylus that wears completely through a film by oscillating or reciprocating back and forth along a linear path until an electrical circuit is completed shutting down the test.  
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Standard Test Method for Detecting Leaks in Nonporous Packaging or Flexible Barrier Materials by Dye Penetration

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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.  
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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.  
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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.  
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5.1 Two procedures, A and B, are outlined in this test method. Procedure A is used most often for development of various beverage container designs to determine the functional characteristics of the package in regard to shelf life. Procedure B is recommended for use in beverage filling operations as a quality control tool in maintaining the desired CO2 fill pressure. A loss of CO2 will affect product taste.  
5.1.1 Procedure A involves the use of sensitive pressure and temperature monitoring equipment where a high degree of accuracy is essential, for example, a micro-pressure transducer and thermocouple for measuring pressure and temperature of the package in a closed system. Alternatively, this procedure may also use bottles closed with roll-on aluminum caps containing rubber septums. The septum is pierced with a hypodermic needle attached to a pressure transducer to obtain pressure readings. This procedure should be confined to laboratories that are practiced in this type of analytical testing.  
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4.2.1 Technique A: Unsuppor...
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1.1 This test method covers the measurement of the strength of seals in flexible barrier materials.  
1.2 The test may be conducted on seals between a flexible material and another flexible material, a rigid material, or a semi-rigid material.  
1.3 Seals tested in accordance with this test method may be from any source, laboratory or commercial.  
1.4 This test method measures the force required to separate a test strip of material containing the seal. It also identifies the mode of specimen failure.  
1.5 This test method differs from Test Method F2824. Test Method F2824 measures mechanical seal strength while separating an entire lid (cover/membrane) from a rigid or semi-rigid round container.  
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1.2 The Precision and Bias statement for this test method was developed using both handheld and bench top micrometers with foot sizes ranging from 4.8 mm to 15.9 mm (3/16 in. to 5/8 in.).  
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5.1 Knowledge of extractives from flexible barrier materials may serve many useful purposes. A test cell constructed as described in this practice may be used for obtaining such data. Another test cell has been found equivalent to the one described in this practice. See the appendix for the source of the alternate cell.  
5.2 United States Federal Regulations 21CFR 176.170 (d)(3), 21CFR 177.1330 (e)(4), 21CFR 177.1360 (b), 21CFR 177.1670 (b), and 21CFR Appendix VI (b) cite this standard practice as the basis for determining the amount of extractables from the surface of a package or multilayer film or modified paper in contact with food. In some cases, it is the only practice defined for this purpose. No alternative detail is given in the regulations for conducting extractions.  
5.3 Test Method D4754 is not an equivalent to this test method. It is for two-sided extraction of films having the same material on both of the exposed surfaces of the film.
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Standard Test Methods for Determining Residual Solvents in Packaging Materials

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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.
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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.  
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1.2 The values stated in SI units are to be regarded as standard. The values given in parentheses are for information only.  
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ASTM F2391-22(Test Method)
Standard Test Method for Measuring Package and Seal Integrity Using Helium as the Tracer Gas

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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),  
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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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