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D3985-05 (2010) E1 Standard Test Method For Oxygen

This document outlines the ASTM D3985 standard test method for determining the oxygen gas transmission rate (OTR) through plastic films and sheeting using a coulometric sensor. It details the scope, terminology, apparatus, and procedures necessary for accurately measuring OTR, including the importance of temperature control and the need for representative test specimens. The standard emphasizes that while OTR is a critical factor for packaging performance, it should be used alongside other tests for comprehensive evaluation.

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0% found this document useful (0 votes)
65 views7 pages

D3985-05 (2010) E1 Standard Test Method For Oxygen

This document outlines the ASTM D3985 standard test method for determining the oxygen gas transmission rate (OTR) through plastic films and sheeting using a coulometric sensor. It details the scope, terminology, apparatus, and procedures necessary for accurately measuring OTR, including the importance of temperature control and the need for representative test specimens. The standard emphasizes that while OTR is a critical factor for packaging performance, it should be used alongside other tests for comprehensive evaluation.

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bendari bendari
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© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Designation: D3985 − 05 (Reapproved 2010)´1

Standard Test Method for


Oxygen Gas Transmission Rate Through Plastic Film and
Sheeting Using a Coulometric Sensor1
This standard is issued under the fixed designation D3985; 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.

ε1 NOTE—Editorial changes were made throughout in November 2010.

1. Scope F1927 Test Method for Determination of Oxygen Gas Trans-


1.1 This test method covers a procedure for determination mission Rate, Permeability and Permeance at Controlled
of the steady-state rate of transmission of oxygen gas through Relative Humidity Through Barrier Materials Using a
plastics in the form of film, sheeting, laminates, coextrusions, Coulometric Detector
or plastic-coated papers or fabrics. It provides for the determi- 3. Terminology
nation of (1) oxygen gas transmission rate (OTR), (2) the
permeance of the film to oxygen gas (PO2), and (3) oxygen 3.1 Definitions:
permeability coefficient (P'O2) in the case of homogeneous 3.1.1 oxygen permeability coeffıcient (P'O2)—the product of
materials. the permeance and the thickness of film. The permeability is
meaningful only for homogeneous materials, in which case it is
1.2 This test method does not purport to be the only method a property characteristic of the bulk material. This quantity
for measurement of OTR. There may be other methods of OTR should not be used, unless the relationship between thickness
determination that use other oxygen sensors and procedures. and permeance has been verified on tests using several different
1.3 The values stated in SI units are to be regarded as thicknesses of the material. The SI unit of oxygen permeability
standard. No other units of measurement are included in this is the mol/(m·s·Pa). The test conditions (see 3.1.3) must be
standard. stated.
1.4 This standard does not purport to address all of the 3.1.2 oxygen permeance (PO2)—the ratio of the OTR to the
safety problems, if any, associated with its use. It is the difference between the partial pressure of O2 on the two sides
responsibility of the user of this standard to establish appro- of the film. The SI unit of permeance is the mol/(m2·s·Pa). The
priate safety and health practices and determine the applica- test conditions (see 5.1) must be stated.
bility of regulatory limitations prior to use. 3.1.3 oxygen transmission rate (OTR)—the quantity of
oxygen gas passing through a unit area of the parallel surfaces
2. Referenced Documents of a plastic film per unit time under the conditions of test. The
SI unit of transmission rate is the mol/(m2·s). The test
2.1 ASTM Standards:2 conditions, including temperature and oxygen partial pressure
D1434 Test Method for Determining Gas Permeability Char- on both sides of the film must be stated.
acteristics of Plastic Film and Sheeting 3.1.3.1 A commonly used unit of OTR is the cm3 (STP)/
D1898 Practice for Sampling of Plastics (Withdrawn 1998)3 (m2·d) at one atmosphere pressure difference where 1 cm3
E691 Practice for Conducting an Interlaboratory Study to (STP) is 44.62 µmol, 1 atm is 0.1013 MPa, and one day is
Determine the Precision of a Test Method 86.4 × 103s. The OTR in SI units is obtained by multiplying the
value in inch-pound units by 5.160 × 10− 10.
1
This test method is under the jurisdiction of ASTM Committee F02 on Flexible 4. Summary of Test Method
Barrier Packaging and is the direct responsibility of Subcommittee F02.10 on
Permeation. 4.1 The oxygen gas transmission rate is determined after the
Current edition approved Oct. 1, 2010. Published November 2010. Originally sample has equilibrated in a dry test environment. In this
approved in 1981. Last previous edition approved in 2005 as D3985 – 05ε1. DOI: context, a “dry” environment is considered to be one in which
10.1520/D3985-05R10E01.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
the relative humidity is less than 1 %.
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM 4.2 The specimen is mounted as a sealed semi-barrier
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
between two chambers at ambient atmospheric pressure. One
3
The last approved version of this historical standard is referenced on chamber is slowly purged by a stream of nitrogen and the other
www.astm.org. chamber contains oxygen. As oxygen gas permeates through

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States

1
D3985 − 05 (2010)´1

FIG. 1 A Practical Arrangement of Components for the Measurement of Oxygen Transmission Rate Using the Coulometric Method

the film into the nitrogen carrier gas, it is transported to the and some strong oxidizing agents. Exposure to carbon dioxide
coulometric detector where it produces an electrical current, should also be minimized to avoid damage to the sensor
the magnitude of which is proportional to the amount of through reaction with the potassium hydroxide electrolyte.
oxygen flowing into the detector per unit time.
7. Apparatus
5. Significance and Use
7.1 Oxygen Gas Transmission Apparatus, as diagrammed in
5.1 The OTR is an important determinant of the packaging Fig. 1 with the following:
protection afforded by barrier materials. It is not, however, the 7.1.1 Diffusion Cell shall consist of two metal halves,
sole determinant, and additional tests, based on experience, which, when closed upon the test specimen, will accurately
must be used to correlate packaging performance with OTR. It define a circular area. The volume enclosed by each cell half,
is suitable as a referee method of testing, provided that the when clamped, is not critical; it should be small enough to
purchaser and the seller have agreed on sampling procedures, allow for rapid gas exchange, but not so small that an
standardization procedures, test conditions, and acceptance unsupported film which happens to sag or bulge will contact
criteria. the top or bottom of the cell. The diffusion cell shall be
5.2 Limited statistical data on correlations with Test Method provided with a thermometer well for measuring temperature.
D1434 methods are available4; however, the oxygen transmis- 7.1.1.1 O-Ring—An appropriately sized groove, machined
sion rate of a standard reference material (see 12.1) as into the oxygen (or test gas) side of the diffusion cell, retains a
determined manometrically by NIST, is in good agreement neoprene O-ring. The test area is considered to be that area
with the values obtained in the coulometric interlaboratory test established by the inside contact diameter of the compressed
using material from the same manufacturing lot. Thus, this test O-ring when the diffusion cell is clamped shut against the test
method may be used as a referee method. specimen. The area, A, can be obtained by measuring the inside
diameter of the imprint left by the O-ring on the specimen after
6. Interferences it has been removed from the diffusion cell.
6.1 The presence of certain interfering substances in the 7.1.1.2 The nitrogen (or carrier gas) side of the diffusion cell
carrier gas stream may give rise to unwanted electrical outputs shall have a flat raised rim. Since this rim is a critical sealing
and error factors. Interfering substances include free chlorine surface against which the test specimen is pressed, it shall be
smooth and flat, without radial scratches.
4
7.1.1.3 Diffusion Cell Pneumatic Fittings—The diffusion
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:D20-1085. Contact ASTM Customer cell shall incorporate suitable fittings for the introduction and
Service at [email protected]. exhaust of gases without significant loss or leakage.

2
D3985 − 05 (2010)´1
7.1.1.4 It is desirable to thermostatically control the diffu- 8.2 Oxygen Test Gas shall be dry and contain not less than
sion cell. A simple heating or heating/cooling system regulated 99.5 % oxygen (except as provided in 14.11).
to 60.5°C, is adequate for this purpose. A thermistor sensor 8.3 Sealing Grease—A high-viscosity silicone stopcock
and an appropriate control circuit will serve to regulate the cell grease or a high-vacuum grease is required for sealing the
temperature unless measurements are being made close to specimen film in the diffusion cell.
ambient temperature. In this case, it is desirable to provide
cooling capability to remove some of the heat. 9. Precautions
7.1.1.5 Experience has shown that arrangements using mul-
tiple diffusion cells are a practical way to increase the number 9.1 Extended use of the test unit, with no moisture in the gas
of measurements which can be obtained from a coulometric stream, may in some older systems result in a noticeable
sensor. Valving connects the carrier gas side of each individual decrease in output and response time from the sensor (equiva-
diffusion cell to the sensor in a predetermined pattern. Carrier lent to an increase in the calibration factor, Q). This condition
gas is continually purging the carrier gas sides of those cells is due to drying out of the sensor.
that are not connected to the sensor. Either test gas or carrier 9.2 Temperature is a critical parameter affecting the mea-
gas, as is appropriate, purges the test gas chamber of any surement of OTR. Careful temperature control can help to
individual cell. minimize variations due to temperature fluctuations. During
7.1.2 Catalyst Bed—A small metal tube with fittings for testing, the temperature shall be monitored to the nearest
attachment to the inlet on the nitrogen side of the diffusion cell 0.5°C. The average temperature and the range of temperatures
shall contain 3 to 5 g of 0.5 % platinum or palladium catalysts found during a test shall both be reported.
on alumina5 to provide an essentially oxygen-free carrier gas.
9.3 The sensor will require a relatively long time to stabilize
7.1.3 Flowmeter—A flowmeter having an operating range
to a low reading characteristic of a good barrier after it has
from 5 to 100 mL/min is required to monitor the flow rate of
been used to test a barrier such as low-density polyethylene.
the nitrogen carrier gas.
For this reason, materials of comparable gas transmission
7.1.4 Flow Switching Valves—Valves for the switching of
qualities should be tested together.
the nitrogen and test gas flow streams.
7.1.5 Coulometric Sensor—An oxygen-sensitive coulomet- 9.4 Back diffusion of air into the unit is undesirable. Care
ric sensor (see Note 1) operating at an essentially constant should therefore be taken to ensure that there is a flow of
efficiency shall be used to monitor the quantity of oxygen nitrogen through the system at all times. This flow can be low
transmitted. when the instrument is not being used.
NOTE 1—It is deemed advisable upon initial setup of the voltage 9.5 Elevated temperatures can be used to hasten specimen
recorder and periodically thereafter to check the response of the recorder outgassing, provided that the treatment does not alter the basic
on all ranges to a suitable voltage input. structure of the specimen (crystallinity, density, and so forth).
7.1.6 Load Resistor—The current generated by the coulo- This can be accomplished by the use of the heaters in the
metric cell shall pass through a resistive load across which the diffusion cells.
output voltage is measured. Typical values for the load resistor
are such that the values yield a convenient relationship between 10. Sampling
the output voltage and the oxygen transmission rate in standard 10.1 The sampling units used for the determination of OTR
units cm3(STP)/(m2·d). shall be representative of the quantity of product for which the
7.1.7 Voltage Recorder—A multirange, potentiometer strip data are required, in accordance with Practice D1898. Care
chart recorder may be used for measuring the voltage devel- shall be taken to ensure that samples are representative of
oped across the load resistor. The recorder should be capable of conditions across the width and along the length of a roll of
measuring a full-scale voltage of 50 mV. It should be capable film.
of measuring voltages as low as 0.100 mV and have a
resolution of at least 10 µV. An input impedance of 1 megohm 11. Test Specimens
or higher is acceptable.
11.1 Test specimens shall be representative of the material
8. Reagents and Materials being tested and shall be free of defects, including wrinkles,
creases, and pinholes, unless these are a characteristic of the
8.1 Nitrogen Carrier Gas shall consist of a nitrogen and
material being tested.
hydrogen mixture in which the percentage of hydrogen shall
fall between 0.5 and 3.0 volume %. The carrier gas shall be dry 11.2 Average thickness shall be determined to the nearest
and contain not more than 100 ppm of oxygen. A commercially 2.5 µm (0.0001 in.), using a calibrated dial gage (or equivalent)
available mixture known as “forming gas” is suitable. at a minimum of five points distributed over the entire test area.
Maximum, minimum, and average values shall be recorded.
11.3 If the test specimen is of an asymmetrical construction,
5
The sole source of supply of the catalyst known to the committee at this time the two surfaces shall be marked by appropriate distinguishing
is Englehard Industries Division, Chemical Dept., 429 Delancey Street, Newark, NJ
marks and the orientation of the test specimen in the diffusion
07105. If you are aware of alternative suppliers, please provide this information to
ASTM International Headquarters. Your comments will receive careful consider- cell shall be reported (for example, “side II was mounted
ation at a meeting of the responsible technical committee,1 which you may attend. facing the oxygen side of the diffusion cell”).

3
D3985 − 05 (2010)´1
12. Calibration materials to a condition where their measured OTRs will be
12.1 General Approach—The oxygen sensor used in this reproducible. Previous experience should serve as the primary
test method is a coulometric device that yields a linear output guide to the suitability of a given conditioning regimen. If a
as predicted by Faraday’s Law. In principle, four electrons are material is being tested with which the user has no previous
produced by the sensor for each molecule of oxygen that passes experience, the effect of conditioning time should be investi-
into it. Considering that the sensor is known to have a basic gated and a regimen selected such that there is no significant
efficiency of 95 to 98 %, it may be considered an “intrinsic” effect due to conditioning time. In any case, the conditioning
standard6 that does not require calibration, and can thus be procedure used should be included in the report section.
used as a reference method. 13.2 Measure OTR in a temperature-controlled environment
12.2 Experience has shown, however, that under some with the apparatus placed in a draft-free location.
circumstances the sensor may become depleted or damaged to 14. Procedure
the extent that efficiency and response are impaired. For that
14.1 Preparation of Apparatus—If preceding tests have
reason, this test method incorporates means for a periodic
exposed the apparatus to high moisture levels, it will be
sensor evaluation. This evaluation is derived from measure-
necessary to outgas the system, particularly the catalyst bed, to
ments of a known-value “reference package.” Experience
desorb residual moisture. Water shall be removed from the
indicates however, that a specimen-to-specimen variability of
nitrogen and test gas humidifiers. The system can then be dried
the reference material7 is such that a change should never be
by slowly purging overnight using dry carrier gas and with the
made in the calibration factor, as the result of a measurement
sensor bypassed. Heating the apparatus will speed the drying
using a single sheet of the reference material.
and outgassing process.
12.3 Establishing a System Calibration Constant (Used only 14.2 Inserting the Specimen—With the sensor bypassed,
on systems using a chart recorder to determine OTR)— unclamp the diffusion cell and open it. Apply a thin layer of
Determine the exposed area, A, of the calibrating reference film sealing grease (see 8.3) around the raised rim of the lower half
(see 7.1.1.1). Using the permeance value furnished with the of the diffusion cell. Remove the test specimen from the
reference film, determine the OTR through that film of that desiccator and place it upon the greased surface, taking care to
area (A). Use this value to determine the calibration constant, avoid wrinkles or creases. Set the movable half of the diffusion
Q: cell into place and clamp both halves tightly together.
OTR 3 R L
Q5 (1) 14.3 Purging the System—Place the system in the CAR-
Ee 2 Eo RIER PURGE mode and purge air from the upper and lower
where: diffusion cell chambers, using a flow rate of 50 to 60 mL. After
OTR = Oxygen transmission rate through a film of area, A, 3 or 4 min, reduce the flow rate to the desired value between 5
as calculated from data supplied with the reference and 15 mL/min. Maintain this configuration for 30 min.
film, 14.4 Establish E0—After the system has been flushed with
RL = value of load resistance, nitrogen for 30 min, INSERT THE SENSOR so that the carrier
Eo = observed steady-state zero-level before oxygen gra- gas which has passed through both sides of the diffusion cell is
dient is applied, and, diverted into the sensor.
Ee = observed steady-state voltage with oxygen gradient
NOTE 2—Eo often is referred to as “individual zero.”
across test film.
At this time, the sensor output will usually increase abruptly,
Repeat the calibration using additional sheets of the refer-
indicating that oxygen is entering the sensor with the carrier
ence film until the confidence interval for Q defined by the
gas. The most likely sources of this oxygen are (1) outgassing
measurements is within acceptable limits.
of the sample, (2) leaks in the system, or (3) a combination of
13. Conditioning (1) and (2). The operator shall observe the recorder trace until
the sensor output current stabilizes at a constant value with no
13.1 Trim the test specimen to a size appropriate for the significant trend in either direction. Thick samples may require
diffusion cell in which it will be mounted. In general, this a purge of several hours, or even overnight, before a steady low
means that the seal around the edge of the diffusion cell should value of sensor current is obtained. On older systems, the
not be impaired if the specimen bulges or sags slightly. After sensor should be bypassed except for brief periods when the
trimming, condition the specimens in a desiccator over calcium zero level is being checked. Once a steady low value of sensor
chloride or another suitable desiccator for a minimum of 48 h. current has been obtained, the sensor may be inserted to
This does not imply that 48 h will be sufficient to bring all monitor the zero level and left there until a stable zero level is
obtained. At this time, the zero level is recorded and labelled
6
Eo. It has been found helpful to periodically test the OTR of a
Garner, E. L., and Raspberry, S. D., “What’s new in Traceability,” Journal of
Testing and Evaluation, Vol 21, No. 6, November 1993, pp. 505–509.
piece of brass shim stock in order to ascertain that no leaks or
7
The sole source of supply of the reference material known to the committee at contamination of the carrier gas have developed.
this time is Mocon, Inc., 7500 Mendelssohn Ave. N, Brooklyn Park, MN 55428. If
you are aware of alternative suppliers, please provide this information to ASTM
14.5 Once E0 has been established, switch OXYGEN into
International Headquarters. Your comments will receive careful consideration at a the test-gas side of the diffusion cell. This action will be
meeting of the responsible technical committee,1 which you may attend. automated on newer systems.

4
D3985 − 05 (2010)´1
14.6 The sensor output current should increase gradually, ~ E e 2 E o! 3 Q
OTR 5 (2)
ultimately stabilizing at a constant value. While some thin A 3 RL
films with high diffusion coefficients may reach equilibrium in
where:
30 to 60 min, thicker or more complex structures may require
a number of hours to reach a steady state of gas transmission. Ee = steady-state voltage level (see 14.6),
The steady-state voltage value of the oxygen transmission rate Eo = zero voltage level (see 14.4),
A = specimen area (see 7.1.1.1),
shall be recorded and labelled Ee.
Q = calibration constant (see Section 12), and
NOTE 3—If, after attainment of an apparent steady-state condition, any RL = value of load resistance (see 7.1.6).
doubt exists as to whether this is a true steady-state condition, perform a Newer, computer-controlled systems will automatically re-
check as follows: (1) bypass the sensor; (2) allow the unit to stabilize for
an additional period of time (minimum of 6 h); and, (3) insert the sensor cord the OTR, and possibly the permeance and permeation
again, and monitor the transmission rate. An increased output indicates coefficient.
that steady-state conditions have not been reached, while the same output 15.2 Determine the permeance (PO2) of the specimen as
(no increase) indicates that steady-state conditions have been initially
obtained. follows:
14.7 Temperature shall be obtained by monitoring the tem- OTR
PO2 5 (3)
perature as close as possible to the specimen. p

14.8 Standby and Shutoff Procedures—Follow the manufac- where p = partial pressure of oxygen, which is the mol
turer’s instructions in the instrument manual for putting the fraction of oxygen multiplied by the total pressure (normally,
instrument into standby mode when the system will not be used one atmosphere), in the test gas side of the diffusion cell. The
for an extended period. partial pressure of O2 on the carrier gas side is considered to be
zero.
14.9 Tests in a Moist Environment—This test method is for
dry (0 RH) conditions only. Specific procedures for testing in 15.3 Determine the oxygen permeability coefficient (P'O2)
a controlled RH environment are covered by Test Method as follows:
F1927. P’O 2 5 PO2 3 t (4)

14.10 The OTR at temperatures other than ambient may be where t = average thickness of the specimen (see 11.2).
determined by thermostatically controlling the diffusion cell Results should be expressed as permeabilities only in cases
provided that the temperature of the carrier gas does not where materials have been determined to be homogeneous by
adversely affect the operation of the sensor. Experience has investigation of the relationship between specimen thickness
shown that the unit can be operated satisfactorily in the range and permeance.
from 4 to 65°C.
16. Report
14.11 Testing Poor Barriers—Films having transmission 16.1 Report the following information:
rates in excess of 200 cm3(STP)/(m2·d) when tested with an 16.1.1 A description of the test specimen, including an
oxygen partial pressure difference of one atmosphere are identification of the two sides of the material if they are
defined as poor barriers. Examples of such materials, depend- different, a statement as to which side was facing the test gas,
ing on thickness, include polyethylene, polycarbonate, and the location of the specimen in the lot of material of which it
polystyrene. High oxygen concentrations in the carrier gas, is representative, and the dimensions of the test specimen.
from the testing of poor barriers, will tend to produce detector 16.1.2 The average thickness of the test specimens as
saturation. One way to avoid this problem is to use a test gas determined in 11.2 and the standard deviation of the thickness
that is a mixture with a known concentration of oxygen in values.
nitrogen. The permeance of the film should be calculated using 16.1.3 The barometric pressure at the time of the test and
the known value of oxygen partial pressure, and then a whether or not barometric pressure compensation is performed
transmission rate should be calculated for the appropriate on the data, either manually or by computer. Barometric
partial pressure difference from the permeance and the desired compensation is performed to standardize data to 760 mm Hg
partial pressure difference. Another way to reduce the oxygen (sea level).
concentration in the carrier gas when testing poor barriers is to
mask off most of the area of the test specimen using a mask of NOTE 4—The barometric compensation factor may be calculated as
follows:
thin metal or aluminum foil on both sides of the test specimen
by use of a suitable adhesive such as contact cement or epoxy. BP760
fBP760 5 (5)
The specimen area then becomes equal to the open area of the BPa
mask. The effect of varying the area of the open hole in the where:
mask should be tested to ensure that the mask is performing fBP760 = barometric compensation factor
properly. BP760 = 760 mm Hg, and
BPa = ambient barometric pressure in mm Hg.
15. Calculation
16.1.4 The partial pressure of the oxygen gas on the test-gas
15.1 If using a chart recorder, determine the OTR as side of the diffusion cell and a statement as to how it was
follows: determined.

5
D3985 − 05 (2010)´1
TABLE 1 Summary of All Test Data
Sample A Sample B Sample C Sample D Sample E Equipment Used
Lab 1 1.120 1.090 0.090 0.062 69.60 73.90 12.20 11.90 0.296 0.293 OxTran Model 2/21 L
Lab 2 1.300 1.260 0.026 0.036 60.50 61.20 12.40 12.30 0.266 0.249 OxTran Model 2/21
Lab 3 1.090 1.050 0.059 0.039 61.23 60.32 12.13 12.02 0.385 0.307 OxTran Model 2/21 H
Lab 4 1.098 1.068 0.048 0.041 70.80 70.50 12.60 12.80 0.310 0.286 OxTran Model 2/21 L
Lab 5 1.140 1.070 0.060 0.060 67.42 75.17 11.82 11.92 0.380 0.350 OxTran Model 2/20
Lab 6 1.090 1.090 0.160 0.180 57.78 56.30 11.07 11.02 0.330 0.340 OxTran Model 702
Lab 7 1.160 1.070 0.050 0.050 58.60 58.30 10.70 11.30 0.260 0.260 OxTran Model 2/21 L
Lab 8 1.12 1.16 0.026 0.025 63.20 65.50 11.80 11.70 0.278 0.285 OxTran Model 2/20 L

TABLE 2 Statistical Summary of Data


Material Average Sr SR r R
Sample A 1.124 0.035 0.071 0.098 0.199
(5.5 mil EVOH
lamination)
Sample B 0.063 0.010 0.047 0.029 0.130
(50 Gage Metalized PET)
Sample C 64.395 2.339 6.269 6.549 17.553
(0.92 mil Mylar)
Sample D 11.856 0.183 0.605 0.512 1.694
(4.75 mil Mylar)
Sample E 0.305 0.022 0.043 0.063 0.120
(5.7 mil EVOH
lamination)

16.1.5 The rate of flow of the nitrogen carrier gas during the Practice E691, involving eight different laboratories measuring
test. five different specimens in duplicate at one test condition. Four
16.1.6 The conditioning procedure used on the test speci- models of a commercially available coulometric gas
mens prior to testing. transmission-measuring instrument were used to collect this
16.1.7 The temperature of the test specimen (to the nearest information. No significant difference was found between
0.5°C) and the method used to determine the temperature. results obtained from the four models, and the results from the
16.1.8 The values of OTR, permeance (if desired), and the four models were pooled together. All measurements made
permeability (if desired). were in units of Oxygen Transmission Rate (cc/(m2-day)) at the
16.1.9 A description of the apparatus used including, if conditions of 23°C, 100 % dry Oxygen test gas gradient. All
applicable, the manufacturer’s model number and serial num- values are normalized to a barometric pressure of one atmo-
ber. sphere. All test data has been summarized in Table 1. Statistical
16.1.10 The calibration factor (Q) and a statement of the
summaries of repeatability (within laboratories) and reproduc-
means used to obtain the calibration factor (only needed if a
ibility (between laboratories) are listen in Table 2.
voltage recorder is being used to calculate OTR).
16.1.11 The effective area for permeation, A, and a descrip-
tion of how it was obtained. 18. Keywords
16.1.12 The time to reach steady-state after introduction of 18.1 coulometric; oxygen transmission rate; permeability;
the oxygen gas into the test-gas side of the diffusion cell. permeation; plastic films
17. Precision and Bias
17.1 A research report (RR:F02-1021 and RR:F02-1022)8
describes a round robin conducted in 2004 in accordance with

8
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Reports RR:F02-1021 and RR:F02-1022.
Contact ASTM Customer Service at [email protected].

6
D3985 − 05 (2010)´1
ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
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make your views known to the ASTM Committee on Standards, at the address shown below.

This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
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