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: F1307 − 20

Standard Test Method for

Oxygen Transmission Rate Through Dry Packages Using a
Coulometric Sensor1
This standard is issued under the fixed designation F1307; 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 3.1.1 oxygen gas transmission rate (O2GTR)—as applied to

1.1 This test method covers a procedure for the determina- a package, is the quantity of oxygen gas passing through the
tion of the steady-state rate of transmission of oxygen gas into surface of the package (PKG) per unit of time.
packages. More specifically, the method is applicable to 3.1.1.1 Discussion—The SI unit of transmission rate is the
packages that in normal use will enclose a dry environment. mol/s. The test conditions, including temperature, oxygen
partial pressure and humidity on both sides of the package,
1.2 The values stated in SI units are to be regarded as the must be stated. A commonly used unit of O2GTR is the
standard. cm3(STP)/(PKG·d), where 1 cm3 at Standard Temperature and
1.3 This standard does not purport to address all of the Pressure (STP = 273.15K; 1.013 × 105 Pa) is 44.62 × 10−6 mol
safety concerns, if any, associated with its use. It is the and one day is 86 400 s. Note: The term package (PKG) is
responsibility of the user of this standard to establish appro- utilized within the transmission rate unit to distinguish it from
priate safety, health, and environmental practices and deter- traditional film OTR results. Unlike film testing, where the test

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mine the applicability of regulatory limitations prior to use.
1.4 This international standard was developed in accor-
area is always known, a package oxygen transmission rate
measurement often involves complex systems with seals and
dance with internationally recognized principles on standard- closures (for example, a bottle with cap, a tray with lidding or
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ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
a heat-sealed foil pouch with permeation through the edges),
where oxygen transmission is occurring. A package OTR test is

Barriers to Trade (TBT) Committee. Document Preview

mendations issued by the World Trade Organization Technical often a packaging “system” test versus a simple component
test.
3.1.2 oxygen permeability coeffıcient (P’O2)—the product of
2. Referenced Documents
ASTM F1307-20
the permeance and thickness of the barrier.
2.1 ASTM Standards:2 3.1.2.1 Discussion—The permeability is meaningful only
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D1434 Test Method for Determining Gas Permeability Char- for homogenous materials, in which case it is a property
acteristics of Plastic Film and Sheeting characteristic of the bulk material. This quantity should not be
D3985 Test Method for Oxygen Gas Transmission Rate used unless the relationship between thickness and permeance
Through Plastic Film and Sheeting Using a Coulometric has been verified in tests using several thicknesses of the
Sensor material. The SI unit of permeability is the mol/(m·s·Pa). The
E691 Practice for Conducting an Interlaboratory Study to test conditions must be stated.
Determine the Precision of a Test Method 3.1.3 oxygen permeance (PO2)—the ratio of the O2GTR to
the difference between the partial pressure of O2 on the two
3. Terminology sides of the package wall.
3.1 Definitions of Terms Specific to This Standard: 3.1.3.1 Discussion—The SI unit of permeance is the mol/
(s·Pa). The test conditions (see 4.2) must be stated.

1
4. Summary of Test Method
This test method is under the jurisdiction of ASTM Committee F02 on Primary
Barrier Packaging and is the direct responsibility of Subcommittee F02.10 on 4.1 This test method employs a coulometric oxygen sensor
Permeation. and associated equipment in an arrangement similar to that
Current edition approved June 1, 2020. Published July 2020. Originally approved
described in Test Method D3985. Oxygen gas transmission rate
in 1990. Last previous edition approved in 2014 as F1307 – 14. DOI: 10.1520/
F1307-20. (O2GTR) is determined after the package has been mounted on
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or a test fixture and has equilibrated in the test environment.
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on 4.2 The package is mounted in such a way as to provide that
the ASTM website. the inside of the package is slowly purged by a stream of

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1
 F1307 − 20
7.1.1.1 Experience has shown that arrangements using mul-
tiple package test stations are a practical way to increase the
number of measurements that can be obtained from a coulo-
metric sensor. A valving manifold connects the carrier gas side
of each individual test station to the sensor in a predetermined
pattern. Carrier gas is continually purging the carrier gas sides
of those packages that are not connected to the sensor. Either
test gas (100 % oxygen) or normal room air (20.8 % oxygen),
whichever is appropriate, contacts the outside of the package.
7.1.2 Diffusion Cell, consisting of two metal halves which,
when closed upon the film used for system calibration, will
accurately define a circular area of that film. Typical diffusion
cell areas are 100 cm2 and 30 cm2. The volumes inside the cell
above and below the enclosed film are not critical; they should
be small enough to allow for rapid gas exchange, but not so
small that an unsupported film which happens to sag or bulge
will contact the top or bottom of the cell. Means shall be
provided for the measurement of cell temperature.
7.1.2.1 O-Ring—An appropriately sized groove, machined
into the oxygen (or test gas) side of the diffusion cell, retains a
neoprene O-ring. The test area is considered to be the area
established by the inside contact diameter of the compressed
FIG. 1 Arrangement of Components when Reference Film is O-ring when the diffusion cell is clamped shut against the test
Used to Calibrate System for Package Testing
specimen. The area, A, can be obtained by measuring the inside
diameter of the imprint left by the O-ring on the specimen after
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nitrogen while the outside of the package is exposed to a
known concentration of oxygen. The package may be exposed
it has been removed from the diffusion cell.
7.1.2.2 The nitrogen (or carrier gas) side of the diffusion cell

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in ambient room air which contains 20.8 % oxygen, or im-
mersed in an atmosphere of 100 % oxygen. As oxygen perme-
shall have a flat raised rim. Since this rim is the sealing surface
against which the test specimen is pressed, it must be smooth

Document Preview
ates through the package walls into the nitrogen carrier gas, it and flat, without scratches which may promote leakage.
is transported to the coulometric detector where it produces an 7.1.2.3 Diffusion Cell Pneumatic Fittings—Each half of the
electrical current, the magnitude of which is proportional to the diffusion cell shall incorporate suitable fittings for the intro-
amount of oxygen flowing into the detector per unit of time. duction and exhaust of gas without significant loss or leakage.
ASTM F1307-20 7.1.2.4 It is desirable to thermostatically control the diffu-
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Significance and Use sion cell. A simple resistive heater, attached to the carrier gas
5.1 Oxygen gas transmission rate is an important determi- side of the cell in such a manner as to ensure good thermal
nant of the protection afforded by barrier materials. It is not, contact, is adequate for this purpose. A thermistor sensor and
however, the sole determinant, and additional tests, based on an appropriate control circuit will serve to regulate the cell
experience, must be used to correlate package performance temperature unless measurements are being made close to
with O2GTR. This test method is suitable as a referee method ambient temperature. In this case, it is desirable to provide
of testing, provided that the user and source have agreed on cooling coils to remove some of the heat.
sampling procedures, standardization procedures, test 7.1.3 Catalyst Bed, a small metal tube with fittings for
conditions, and acceptance criteria. attachment to the inlet of the nitrogen gas pneumatic fitting
containing 3 to 5 g of 0.5 % platinum or palladium catalyst on
6. Interferences alumina to provide an essentially oxygen-free carrier gas to the
6.1 The presence of certain interfering substances in the diffusion cell and to each package test station.
carrier gas stream may give rise to unwanted electrical outputs 7.1.4 Flowmeter, a flowmeter having an operating range of
and error factors. Interfering substances include free chlorine 5 to 100 mL/min is required to monitor the flow rate of
and some strong oxidizing agents. Exposure to carbon dioxide nitrogen carrier gas through each test station.
should also be minimized to avoid damage to the sensor 7.1.5 Flow Switching Valves—Two or more valves for the
through reaction with the potassium hydroxide electrolyte. switching of the nitrogen and test gas flow streams.
7.1.6 Oxygen-Sensitive Coulometric Sensor, operating at an
7. Apparatus essentially constant efficiency is employed to monitor the
7.1 Oxygen Gas Transmission Apparatus, as diagrammed in quantity of oxygen transmitted.
Fig. 1 with the following: 7.1.7 Load Resistor—The current generated by the coulo-
7.1.1 Package Test Stations, providing a means for the metric cell shall pass through a resistive load across which the
introduction and exhaust of the nitrogen carrier gas stream output voltage is measured. Typical values for load resistors are
without significant loss or leakage. such that the values yield a convenient relationship between the

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 F1307 − 20
output voltage and the oxygen transmission rate as expressed in 11. Test Specimens
terms of cm3(STP)/(PKG·d).
11.1 Test packages shall be representative of the population
7.1.8 Voltage Recorder—The voltage across the load resis-
and shall be free of non-typical defects, unless these defects are
tor is measured and recorded using a strip-chart potentiometer,
a characteristic of the package being analyzed (for example,
data-logger or other suitable device. The instrument or system
wrinkled pouch, dented bottle...etc.)
should be able to measure a full-scale voltage of 50 mV. It
should be able to measure voltages as low as 0.10 mV with a
12. Calibration
resolution of at least 10 µV. An input impedance of 5000 ohm
or higher is acceptable. 12.1 General Approach—The oxygen sensor used in this
method is a coulometric device that yields a linear output as
8. Reagents and Materials predicted by Faraday’s Law. Since this sensor has an efficiency
8.1 Nitrogen Carrier Gas, consisting of a nitrogen and of 95 to 98 % it is almost an absolute “yardstick” that does not
hydrogen mixture in which the percentage of hydrogen shall require calibration. Experience has shown, however, that under
fall between 0.5 and 3.0 volume percent. The carrier gas shall some circumstances the sensor may become depleted or
be dry and contain not more than 100 ppm of oxygen. A damaged to the extent that efficiency and response are im-
commercially available mixture known as “forming gas” is paired. For this reason, the method incorporates means for
suitable. periodic system calibration. This calibration is derived from
8.2 Sealing Grease—A high-viscosity silicone stopcock measurements of a known-value “Reference Package.”
grease or a high-vacuum grease is required for sealing the 12.2 The reference package is essentially the lower-half of a
calibration film in the diffusion cell. diffusion cell (Fig. 1) in which a sheet of reference film of
8.3 Oxygen Test Gas—The test gas shall be dry and contain known O2GTR has been sealed and clamped. This creates a
not less than 99.5 % oxygen (except as provided for in 14.8). “package” into which oxygen will diffuse at a known rate.
9. Technical Precautions 12.3 Assembling the Reference Package—Ensure the sensor
is bypassed to avoid swamping it with air, that is, no flow to the
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9.1 Extended use of the test unit with no moisture in the gas sensor. Unclamp the diffusion cell and open it. Apply a thin
stream may result in a noticeable decrease in output and layer of sealing grease (see 8.2) around the raised rim of the
response time from the sensor (equivalent to an increase in the
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lower half of the diffusion cell. Insert the reference film in the
calibration factor, Q). This condition is due to drying out of the diffusion cell and place it upon the greased surface, taking care
sensor. to avoid wrinkles or creases. Lower the upper half of the
Document
surement of O GTR. Careful temperature
2 control can help to Preview
9.2 Temperature is a critical parameter affecting the mea- diffusion cell into place and clamp both halves tightly together.
12.4 Purging the System—Start the nitrogen carrier gas flow
minimize variations due to temperature fluctuations. During
and purge air from the upper and lower diffusion cell chambers
testing, monitor and record the temperature, periodically, to the
ASTM F1307-20using a flow rate of 50 to 60 cm3/min (as indicated by the
nearest 0.5°C. Report the average temperature and the range of
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temperatures found during a test.
flowmeter). After 3 or 4 min, reduce the flow rate to the desired
value between 5 and 15 cm3/min. Maintain this configuration
9.3 The sensor will require a relatively long time to stabilize for 30 min.
at a low reading characteristic of a good barrier after it has been
used to test a barrier such as low-density polyethylene. For this 12.5 Establishing Zero Level of Reference Film—After the
reason, materials of comparable gas transmission qualities system has been flushed with nitrogen for 30 min, with the
should be tested together. sensor bypassed, divert the nitrogen carrier gas flow to the
sensor. At this time the sensor output, as displayed on the
9.4 Back diffusion of air into the unit is undesirable. Take voltage recorder, will usually increase abruptly, indicating that
care, therefore, to ensure that there is a flow of nitrogen oxygen is entering the sensor with the carrier gas. The most
through the system at all times. This flow can be low when the likely sources of this oxygen are (1) outgassing of the sample,
instrument is not being used. (2) leaks in the system, or (3) a combination of (1) and (2). The
9.5 The gas-permeability characteristics of some barrier operator shall observe the recorder trace until the sensor output
materials are altered by exposure to water vapor. If a package current stabilizes at a constant low value with no significant
is to be exposed and tested in normal laboratory air (20.8 % trend in either direction. Note the observed deflection of the
O2), the ambient relative humidity should be monitored to the strip chart recorder at this time and label it E0.
nearest 3 %. This may be accomplished using a sling psy-
12.6 Once the zero level (E0) has been established, switch to
chrometer or other method of comparable accuracy. Report the
a flow of oxygen on the test gas side of the diffusion cell.
average and range of relative humidities measured during the
Nitrogen will continue to flow on the downstream side of the
test.
cell.
10. Sampling 12.7 Establishing a Steady-State O GTR—The sensor
2
10.1 The sampling units used for the determination of output, as displayed by the strip-chart recorder, should increase
O2GTR shall be representative of the quantity of product for and gradually level off, approaching a constant value (Ee).
which the data are required. Record the observed final steady-state value of Ee.

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 F1307 − 20
12.8 Temperature of the Reference Film—It is desirable that
system calibration should be conducted at the temperature for
which the reference film’s O2GTR is cited. Apply an appro-
priate correction to the rate that the temperature differs from
that value. Temperature shall be obtained by monitoring
thermometers or thermocouples placed in the thermometer
wells on both sides of the reference film. The film temperature
may be assumed to be midway between the two values.
12.9 Standby Procedure—At the conclusion of system
calibration, but when it is expected that package tests will be
performed soon, the instrument should be placed in a standby
condition by taking the following steps: (1) stop the flow of O2
test gas to the sensor, and switch to nitrogen carrier gas on the
test gas side of the diffusion cell, (2) turn off the oxygen supply,
and (3) reduce the nitrogen flow rate to less than 5 mL/min. It
is desirable to maintain a slow flow of nitrogen through the
instrument when it is not being used in order to reduce the back
diffusion of air into the system.
12.10 Establish System Calibration Constant—Determine
the exposed area, A, of the calibrating reference film (see FIG. 2 Typical Method of Attaching a Plastic Bottle or Tub
7.1.2.1). Using the permeance value furnished with the refer-
ence film, determine the O2GTR through a film of that area (A). package shape, type, and test objectives. For a majority of tests,
Use this value to determine the calibration constant, Q : the package may be exposed to ambient air (20.8 % O2). If the
package is an extremely good barrier, however, it may be
O 2 GTR 3 R L

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Q5 (1) helpful to increase the test gradient by immersing the package
~ E e 2 E o! in 100 % oxygen. This is accomplished by securing a plastic
where: bag, pouch overwrap, or other container around the test
O2GTR (https://standards.iteh.ai)
= oxygen transmission rate through a film of area
A, as calculated from data supplied with the
package and flooding the bag with oxygen as shown in Fig. 2.
This will increase the transmission rate by a factor equal to the

= value of load resistanceDocument Preview

reference film, ratio:
RL (see 7.1.7), 100 %
E0 = observed steady-state zero-level before oxygen 5 4.8 (2)
21 %
gradient is applied (see 12.5), and Whenever 100 % oxygen is used to establish the test
Ee = observed steady-state voltage with oxygenASTM F1307-20
gradi- gradient, the operator should use care not to pressurize the
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ent across test film (see 12.7). oxygen-containing structure. (Oxygen partial pressure should
be equal to the prevailing atmospheric pressure.) Pressuriza-
Repeat the calibration using additional sheets of the refer- tion may be avoided by providing a small vent and by in-
ence film until the confidence interval for Q defined by the jecting the oxygen at a low rate on the order of 10 to 20
measurements is within acceptable limits. When operating an mL/min. Bottles, thermoformed plastic cups, and tubs are
instrument with multiple diffusion cells, it is desirable to keep usually mounted as shown in Fig. 2. Flat pouches and bags
a sheet of the reference film in one of the diffusion cells to may be mounted using some variation of Fig. 3. In attaching
ensure the reliability of the rates being measured. a pouch, it is important that the copper tubes first be con-
nected securely to the fittings and then bent to the desired
12.11 In principle, each molecule of oxygen that enters the angles. Corners of the pouch may then be snipped off to pro-
sensor causes the transfer of four electrons. Experience indi- vide openings just large enough for the tubes. After the
cates that production models of the sensors achieve efficiencies package has been slipped over the tube ends, a fast-curing
of 95 to 98 %. Any significant drift in the calibration factor Q epoxy or hot-melt adhesive is carefully applied to seal cut
openings.
should, therefore, be investigated as to its cause and corrective
action should be undertaken. 13.2 The detector output is governed by Faraday’s Law, and
the calibration does not vary with temperature. It should be
12.12 The value of Q will be a function of the units in which
noted, however, that the oxygen transmission rate of most
the results are to be expressed. If it is desired to change units,
plastic materials will vary 3 to 9 % ⁄°C. Since the package test
Q can be transformed to its proper value in the new set of units
attachment does not provide means for control of package
using the appropriate relationships between base units (quan-
temperature, it will prove advantageous from the standpoint of
tity of matter, length, and time) in the new and the old sets of
data reproducibility to locate the instrument in a draft-free,
units.
constant-temperature environment.
13. Preparation of a Package for Test 14. Package Test Procedure
13.1 The method by which a package is prepared for 14.1 Preparation of Apparatus—If preceding tests have
attachment to the instrument for testing depends upon the exposed the apparatus to high moisture levels, it will be