Designation: D 2684 – 95 (Reapproved 2001)

Standard Test Method for

Permeability of Thermoplastic Containers to Packaged
Reagents or Proprietary Products1
This standard is issued under the fixed designation D 2684; 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. Terminology
1.1 This test method covers procedures for determining the 3.1 Definitions:
permeability of thermoplastic containers to packaged reagents 3.1.1 permeability factor, Pt —the permeability of a given
or proprietary products under specified conditions of exposure. plastic to a given product at temperature t, in degrees Celsius,
The exposures used are intended to simulate the normal and expressed in units of g·cm/day·m2, as determined by Procedure
elevated temperature-storage conditions that might be encoun- A. The permeability factor under 23°C test conditions, for
tered in end-use application. example, is signified by the notation P23.
1.2 This test method is applicable only to those types of 3.1.2 Determination of Pt is based on an averaged wall
containers designed to allow positive, leakproof closure. thickness over the entire area of the container and an assump-
1.3 Two procedures are provided: tion that permeation rate is inversely proportional to the
1.3.1 Procedure A is specific to testing only with a standard thickness. Precaution in the extent of allowable variations of
design container. This procedure provides for determinations these factors is recommended, and use of Pt should take into
of rate of weight loss (or gain) and for calculation of a consideration that wall thickness of the containers varies, that
permeability factor. the estimate of average thickness from density, area, and
1.3.2 Procedure B applies to tests of all other container weight is not exact, and that permeability of the product
designs. Permeability data by this procedure are expressed only through the plastic material may not be directly proportional to
in terms of rate of weight loss (or gain) for the particular the thickness.
container tested.
1.4 The values stated in SI units are to be regarded as the 4. Summary of Test Method
standard. 4.1 Test bottles are filled with the test product and, after
sealing, are exposed at 23°C (73.4°F) and 50°C (122°F)
NOTE 1—There is no similar or equivalent ISO Standard.
conditions for 28 days or longer. Measurements of weight are
1.5 This standard does not purport to address all of the made at intervals to determine the average rate of weight
safety concerns, if any, associated with its use. It is the change.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica- 5. Significance and Use
bility of regulatory limitations prior to use. 5.1 With the proper precautions and background experience,
results can be useful for estimation of the loss of a packaged
2. Referenced Documents
product through the walls of a container during shelf storage.
2.1 ASTM Standards: The test is also useful for isolating the effects of a container
D 618 Practice for Conditioning Plastics for Testing2 design and materials, and is applicable for development and
D 1248 Specification for Polyethylene Plastics and Extru- research and for specification purposes.
sion Materials for Wire and Cable2 5.2 In the absence of adequate supporting data, extrapola-
D 1505 Test Method for Density of Plastics by the Density- tions or correlations of results to conditions beyond those of the
Gradient Technique2 test are not recommended because of possible product alter-
E 145 Specification for Gravity-Convection and Forced- ation, solvency, or chemical effects on the plastic, etc.
Ventilation Ovens3 5.3 Before proceeding with this test method, reference
should be made to the specification of the material being tested.
1
Any test specimen preparation, conditioning, dimensions, or
This test method is under the jurisdiction of ASTM Committee D20 on Plastics
and is the direct responsibility of Subcommittee D20.20 on Plastic Products. testing parameters, or combination thereof, covered in the
Current edition approved Nov. 10, 1995. Published January 1996. Originally materials specification shall take precedence over those men-
published as D 2684 – 68 T. Last previous edition D 2684 – 89. tioned in this test method. If there are no material specifica-
2
Annual Book of ASTM Standards, Vol 08.01.
3
Annual Book of ASTM Standards, Vol 14.02.
tions, then the default conditions apply.

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

1
 D 2684
6. Apparatus
6.1 Enclosure or room with provision for maintaining the
standard laboratory atmosphere of 23 6 2°C (73.4 6 3.6°F)
and 50 6 5 % relative humidity, as defined by Practice D 618.
6.2 Circulating-Air Oven, consistent with ovens in accor-
dance with Specification E 145, capable of maintaining a
temperature of 50 6 1°C (1226 1.8°F) and an airflow rate of
8.5 to 17.0 m3 /min (300 to 600 ft3 /min). The limitation of 25
ft3 on oven size can be overlooked, provided all other require-
ments are met.
NOTE 2—Only explosion-proof equipment with provision for adequate
exhaust of vapors should be used for tests with potentially hazardous or
toxic products.
NOTE 3—Relative humidity variation can significantly affect perme-
ability loss in many products, especially water-based products in various
thermoplastics. Therefore, the user may find it useful to equip the oven
with a means to measure relative humidity and to record the same during
the period of test.
6.3 Balance, accurate to 0.01 % of the weight of test
container and contents.
6.4 Container Seals, suitable heat-sealing laminate4 and
polyethylene or other suitably lined screw-type closures for
sealing the containers. NOTE 1—Dimensions are in millimetres.
6.5 Heat Sealer.5 FIG. 1 Standard Container for Permeability Test
6.6 Torque Wrench.6
In cases of disagreement, the tolerances shall be 6 1°C
7. Reagents and Materials (61.8°F) and 62 % relative humidity.
7.1 The reagent or proprietary product as specified for 9.2 Test Conditions—Conduct tests in the standard labora-
testing. tory atmosphere of 23 6 2°C (73.4 6 3.6°F) and 50 6 5 %
relative humidity, unless otherwise specified in the test meth-
8. Test Specimens ods. In cases of disagreements, the tolerances shall be 61°C
8.1 The test specimen for Procedure A shall be the 4-oz (61.8°F) and 62 % relative humidity.
cylindrical bottle design as specified in Fig. 1, having a
10. Procedure A (Standard Container)
nominal external surface area of 154 cm2 (23.8 in.2).
8.2 The test specimen for Procedure B may be any thermo- 10.1 With specimens taken from the sidewalls of three of
plastic container, as specified or selected for test evaluation, the containers, determine the average plastic density by Test
provided it is designed to allow positive closure. Method D 1505, or by an alternative method of equivalent
8.3 For each procedure, a minimum of three specimens shall accuracy.
be tested at each temperature. Three additional specimens are 10.2 For each test temperature, select a minimum of three
required for Procedure A for determination of the plastic containers. Weigh each when empty, without the closure. Also
density. weigh the empty containers with their corresponding closures
and appropriately sized laminate pieces.
NOTE 4—Trim and finish the containers, if needed, to ensure a smooth 10.3 Fill the containers to nominal capacity with the test
contacting surface for positive seal.
product.
9. Conditioning 10.4 Make a thorough check for any drippage or spill of
product on the outside surface of the containers. If any is noted,
9.1 Conditioning—Condition the test specimens at 23 6
replace the container with a new specimen.
2°C (73.4 6 3.6°F) and 50 6 5 % relative humidity for not less
10.5 Heat seal the containers with the laminate (plastic to
than 40 h prior to test in accordance with Procedure A of
plastic), check for leaks, and then cap the containers with
Practice D 618, for those tests where conditioning is required.
screw-type closures, using sufficient torque to provide positive
seal. Avoid distorting the container when capping.

4
NOTE 5—One method of testing for a poor seal is to immerse an upright
One such laminate suitable for polyethylene containers, MIL-B-131C Class 2, test container in a beaker filled to the base of the cap with a liquid that will
a polyethylene-aluminum foil-paper laminate available from the Robertson Co.,
not attack the plastic. When a vacuum of 15 in. Hg is applied to the entire
Jamaica, NY. Heat sensitive seals are also available from 3M Packaging Systems
Division, 3M Center Building 220-8W-01, St. Paul, MN, 55144.
system, a poorly sealed bottle will give off bubbles from the sealed area.
5
Super Sealer made by Ciamco Corp., 12900 Plaza Dr., Cleveland, OH 44130 NOTE 6—Any deformation of the container during sealing may result in
is suitable. a volume change which will affect the final test pressure. An application
6
Model 25 Owens-Illinois Torque Tester, Model MRA available from Secure torque of 1.7 N·m (15 lbf·in.) has been found sufficient for the standard
Pak, Inc., P.O. Box 14499, Toledo, OH 43614 is suitable. container in Fig. 1.

2
 D 2684
10.6 Weigh the sealed containers.
10.7 Unless otherwise specified, expose one set of contain- R = rate of average weight change, g/day, from 10.9.2, and
ers in the Standard Laboratory Atmosphere, 23 6 2°C (73.4 6 T = average bottle wall thickness, cm, calculated from
3.6°F) and 50 6 5 % relative humidity, and another set in a bottle weight, area in cm2, and density of the bottle
circulating-air oven controlled at 50 6 1°C (122 6 1.8°F). material, for example:
Place the containers upright on an inert metal screen or weight of bottle ~g!
perforated sheet support to allow air circulation. Place a tray T 5 (5)
density ~g/cm 3! 3 area ~cm 2!
beneath the container support to collect leakage of product, if
failure occurs. Provide enough spacing between the containers
so they do not touch each other. Also, take precautions as A = bottle surface area, m2.
necessary to prevent any possible cross-contamination in the
NOTE 8—For Procedure A, where the standard 4-oz Boston Round
test chamber from other agents. Bottle is used (23.8-in.2 area), the following equations can be used:
NOTE 7—For certain relatively unstable or spoilable products, the use To calculate Pt in metric units:
of elevated temperature exposures may not be applicable. RT/A 5 R ~g/day! 3 weight of bottle ~g!
Pt 5 (6)
10.8 Weigh the containers after 1 day, 7 days, 14 days, 21 density ~g/cm3! 3 2.358
days, and 28 days. In certain cases, a steady rate of weight
change may be reached in either a shorter or longer period. 11. Procedure B (Nonstandard Containers)
Other intervals can then be used. They should be regular and 11.1 Follow the procedure in 10.2-10.8.
reported.
NOTE 9—If not feasible to heat seal the container due to design, etc.,
10.8.1 If the weight change appears abnormal for any of the any other means for providing an equivalent, nonpermeable, leakproof
containers during exposure, inspect the containers to ensure closure would be an acceptable alternative.
that a positive seal exists. If a leak is detected, retest with a new
11.2 Calculation:
specimen.
11.2.1 Calculate the percentage weight loss or gain after a
10.8.2 Cool in the standard laboratory atmosphere until
given exposure time as detailed in 10.9.1.
consistent weighings are obtained. Resume oven exposure
11.2.2 Calculate the rate of average weight change as shown
within 6 h from removal time.
in 10.9.2.
10.8.3 In elevated-temperature tests, rotate the locations of
the specimens in the oven when re-exposing after each interval 12. Report
to minimize possible bias due to variations of airflow and
temperature within the oven. 12.1 Report the following information:
10.9 Calculation: 12.1.1 Complete bottle and test product identification and
10.9.1 Calculate the percentage weight loss or gain after a description,
given exposure time as follows: 12.1.2 Complete closure identification and description.
12.1.3 Exposure conditions,
Weight loss ~at time x!, % 5 @~Gu 2 Gx!/Nu # 3 100 (1)
12.1.4 Calculated permeation data,
Weight gain ~at time x!, % 5 @~Gx 2 Gu!/Nu # 3 100 (2) 12.1.5 Any occurrences of container leakage, failure, etc.,
12.1.6 Date of test,
where:
12.1.7 Duration of test, and
Gu = gross weight of unexposed bottle, closure, and
12.1.8 Regular weighing intervals.
contents, g,
Gx = gross weight of exposed bottle, closure, and
13. Precision and Bias
contents, g, and
Nu = net weight of unexposed test product in the 13.1 Round-robin testing7 among six laboratories by Proce-
bottle, g. dure A was performed with containers of Type I polyethylene
10.9.2 Rate of Average Weight Change—Plot the weight in accordance with Specification D 1248, and a variety of
changes, Gu − Gx for losses or Gx − Gu for gains, versus time liquid reagents. Pt values ranged from 0.02 to about 200
in days on rectilinear graph paper. Draw the best straight line mg·cm/day·m2. Over this wide range, the standard deviations
through the points, ignoring, if necessary, points near the of the results between laboratories increased with increased
beginning or end of the test period that deviate excessively values of Pt. For 18 levels of Pt, the interlaboratory coefficients
from the best line through intermediate points. From the slope of variation remained relatively constant with the overall
of the line, determine the rate of average weight change, R, in average being 14 %.
grams per day, as illustrated in Fig. 2. Note whether the change 13.2 Since there is no accepted reference method for this
is loss or gain. test method, the bias of this test method cannot be determined.
Weight change per day, % 5 ~R/Nu! 3 100 (3)
14. Keywords
10.9.3 Permeability Factor (see 3.1)—Calculate the perme- 14.1 containers; permeability; plastic bottles
ability factors as follows:
Pt 5 RT/A (4)
2
For Pt in metric units, g·cm/day·m . 7
Supporting data have been filed at ASTM Headquarters. Request RR:D20–50.

3
 D 2684

FIG. 2 Example Plot—Determination of Slope for Rate of Weight Change

APPENDIX

(Nonmandatory Information)

X1. MIXED INCH-POUND METRIC UNITS AND CONVERSION FACTORS

X1.1 For Pt in mixed inch-pound-metric units, g·mil/ NOTE X1.1—The mixed inch-pound-metric units are not recommended
day·100 in.2. for general use, but are included to establish a relationship with work that
has been previously accomplished in this area.

R = rate of average weight change, g/day, from 10.9.2, X1.2 To convert Pt values between systems use the follow-
T = average bottle wall thickness, mil, calculated from ing equations:
bottle weight, area in in.2, and density, for example:
Pt (metric units) = 0.0394 Pt (mixed inch-pound-metric
weight of bottle ~g! 3 1000 ~mil/in.! units)
T 5 (X1.1)
density ~g/cm 3! 3 16.39 ~cm 3! 3 area ~in. 2!
Pt (mixed inch-pound-metric units) = 25.4 Pt (metric units)

A = bottle surface area in units of 100 in.2 ; for example, if

bottle surface area is 23.8 in.2, A = 0.238.

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
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.

4
 D 2684

This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
address or at 610-832-9585 (phone), 610-832-9555 (fax), or service@astm.org (e-mail); or through the ASTM website
(www.astm.org).