Designation: D 5094 04

Standard Test Methods for

Gross Leakage of Liquids from Containers with Threaded or Lug-Style Closures1

This standard is issued under the xed designation D 5094; 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 1.1 These test methods may demonstrate container/closure integrity with threaded or lug-style closures by the determination of gross leaks in rigid and semi-rigid containers (up to 4 L (1.06 g). Such tests may be used to indicate the ability of a liquid container to survive the distribution environment without leaking. These test methods may not be suitable to determine the leak resistance of containers intended for transport of hazardous materials. 1.2 Test Methods: 1.2.1 Test Method A, Shipping Container Vibration and Storage Test, covers the ability of a shipping container and its interior packaging to protect the contents from leakage after transportation induced vibration and high-temperature storage. 1.2.2 Test Method B, Shipping Container Vibration and Vacuum Chamber Test, is suitable for individual containers and is usually less severe than Test Method A. The advantage of Test Method B is the shortness of the test. 1.3 This standard does not purport to address the safety conserns 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. 2. Referenced Documents 2.1 ASTM Standards: 2 D 996 Terminology of Packaging and Distribution Environments D 999 Test Methods for Vibration Testing of Shipping Containers D 3198 Test Method for Application and Removal Torque of Threaded or Lug-Style Closures
1 This test method is under the jurisdiction of ASTM Committee D10 on Packaging and is the direct responsibility of Subcommittee D10.32 on Consumer Packages. Current edition approved April 1, 2004. Published May 2004. Originally approved in 1990. Last previous edition aprpoved in 1990 as D 509490(2003). 2 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 standards Document Summary page on the ASTM website.

D 3474 Practice for the Calibration and Use of Torque Meters Used in Packaging Applications D 4169 Practice for Performance Testing of Shipping Containers and Systems D 4332 Practice for Conditioning Containers, Packages, or Packaging Components for Testing 3. Terminology 3.1 General denitions for packaging are found in Terminology D 996. 3.2 Denitions of Terms Specic to This Standard: 3.2.1 gross leakany opening in the container or closure seal that produces visible leakage such that the container would not be suitable for transport or subsequent distribution. 3.2.2 leakany opening in a container which, contrary to intention, either lets contents escape or permits substances to enter. 3.2.3 leakagethat which passes through a leak. 4. Summary of Test Methods 4.1 Method A, Shipping Container Vibration and Storage TestTest specimens are lled to their expected ll capacity with product or liquid simulating product and the closure is applied to the container. Closures should be applied with the same torque as would be encountered in production. The specimens are packed into shipping containers and vibrated. The specimens, stored on their sides, are subjected to 40C (104F) (or other conditions as appropriate) for four weeks. Each specimen is examined for leakage. 4.2 Method B, Container Vibration and Vacuum Chamber TestTest specimens are partially lled with product or liquid simulating product and the closure is applied to the container. Closures should be applied with the same torque as would be encountered in production. The specimens are packed into shipping containers and vibrated. Following vibration, the individual specimens are removed from the shipping container and subjected to 10 in. Hg (33.7 kPa) vacuum for 10 min and examined for leakage.
NOTE 1Other levels of vacuum, or time, or both may be appropriate.

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5. Signicance and Use 5.1 These test methods are used to indicate the integrity of the container and closure system in the distribution environment. 5.2 These test methods measure the ability of the container and closure system to prevent leakage when stored or transported upright, inverted, or on the side. 5.3 These test methods allow for comparison of container/ closure designs of threaded and lug-style closures of similar or different materials, or different manufacturers. These tests are suitable for packaging development, engineering and tooling evaluations. 6. Apparatus 6.1 Method A, Shipping Container Vibration and Storage Test: 6.1.1 Drying Oven, constant-temperature, equipped with means for ensuring adequate temperature control, 40 6 1C (104 6 1.8F) and air circulation, ambient humidity, or other conditions as appropriate. 6.1.2 Torque Meter, with an appropriate scale which accurately measures within the expected torque range. 6.1.3 Vibration Test Machine, the apparatus described in the Apparatus section of Methods D 999 may be used. 6.2 Method B, Shipping Container Vibration and Vacuum Test: 6.2.1 Vacuum Chamber, any suitable chamber capable of withstanding approximately one atmosphere pressure differential, tted with a vacuum-tight seal. A vacuum gauge, an inlet tube from a source of vacuum, and an outlet tube to the atmosphere shall be sealed to the chamber. The inlet and outlet tubes shall be equipped with shut-off valves. The vacuum gauge shall be laboratory quality with a full scale range of 0 to 30 in. Hg (0 to 100 kPa). 6.2.2 Torque Meter, with an appropriate scale which accurately measures within the expected torque range. 6.2.3 Vibration Test Machine, the apparatus described in the Apparatus section of Methods D 999 may be used. 7. Sampling 7.1 The complete test unit shall consist of the shipping container, with interior packaging and the actual test specimens (container(s) and closure(s)). 7.2 A minimum of three specimens representing each variable, such as cap or bottle mold from each cavity but not less than ten specimens are to be selected. The total number of specimens may need to be increased to completely ll the shipping container. More than one shipping container may be required. 7.3 Select unused closures and unused containers that are within specications. 8. Test Specimens 8.1 Test Method AA specimen shall be one container lled to expected ll capacity with product or liquid simulating product. The closure is secured in accordance with 11.1. 8.2 Test Method BA specimen shall be one container one-third lled with product or liquid simulating product. The closure is secured in accordance with 11.1.
2

8.3 Colorant should be added to the contents when necessary to give permanent indication where there is leakage. 9. Calibration 9.1 Calibrate the torque meter in accordance with Practice D 3474. 10. Conditioning 10.1 Store the shipping container components at ambient laboratory conditions for at least 4 h before testing, or other conditions in accordance with Practice D 4332. 10.2 Store the torqued container/closure test specimens upright at least 24 h at ambient conditions before commencing the test. 11. Procedure 11.1 Apply closures to the containers according to the Application Torque Measurement section of the procedure in Test Method D 3198. 11.2 Test Method A, Shipping Container Vibration and Storage Test: 11.2.1 Place the lled specimens in their shipping container or in an appropriate carton so that they will remain rmly in place during vibration. 11.2.2 Proceed as directed according to Methods D 999 (Method A 1 or A 2) 20 min each on bottom, top, and one side, or run an entire shipping cycle in accordance with Practice D 4169. 11.2.3 Remove the specimens from the shipping container or carton. Examine all specimens for visible leakage without removing or disturbing the closure. Note the location(s) of leakage. 11.2.4 Place the test specimens on their sides (liquid in contact with nish/closure) in a container capable of holding the liquid should a leak develop. It is recommended that absorbent blotting paper be placed beneath the samples to more easily detect leakage. Store the test specimens at 40 6 1C (104 6 1.8F), or other appropriate temperature, ambient humidity and inspect for liquid leakage at 24 h and at one-week intervals for four weeks. Note location(s) of leakage. 11.2.5 At the conclusion of the test, remove the closure and inspect the threads for signs of leakage or crusting from partial leakage. 11.3 Test Method B, Shipping Container Vibration and Vacuum Chamber Test: 11.3.1 Place the partially lled specimens in their shipping container or in an appropriate carton so that they will remain rmly in place during vibration. 11.3.2 Proceed as directed according to Methods D 999 (Method A 1 or A 2) 20 min each on bottom, top, and one side, or run an entire shipping cycle in accordance with Practice D 4169. 11.3.3 Remove the specimens from the shipping containers or carton. Examine all specimens for visible leakage without removing or disturbing the closure. Note location(s) of leakage. 11.3.4 Place the partially lled specimens inverted in a beaker or other receptable to contain leakage.
NOTE 2Other orientations of the specimens may be appropriate.

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Orientation of the container should be such that suspected leak areas are covered with the liquid inside the container.

11.3.5 Place specimens in the vacuum chamber and close the vacuum chamber. 11.3.6 Close the chamber inlet valve. 11.3.7 Open the chamber outlet valve and turn on vacuum source so that the gauge rises slowly (from 30 s to 1 min) to 10 in. Hg (33.7 kPa) and close the outlet valve. 11.3.8 Maintain the vacuum for 10 min. 11.3.9 Partially open the chamber inlet valve and release the vacuum slowly (30 s to 1 min). 11.3.10 Open the chamber. 11.3.11 Remove the specimens and examine for leakage, cracks, or other visible damage. Record the results of this examination. Note location(s) of leakage. 12. Interpretation of Results 12.1 If there is leakage to the outside of the specimen, the package fails the test. 12.2 If there is no leakage to the outside of the specimen the package passes the test. 12.3 If there is leakage to the threads but not to the outside, the specimen may or may not be acceptable. This effect may be used as a comparative evaluation between closures and mold cavities. 13. Report 13.1 Report the following information:

13.1.1 Statement that testing was done in accordance with ASTM Test Method D 5094, Test Method A or Test Method B, or that the testing was done with indicated changes. 13.1.2 Materials of construction of the closure, liner and container including nish and manufacturers designation. 13.1.3 Description of the shipping container and interior packaging, the test frequencies, intensities, and durations used. 13.1.4 Product or substitute used and ll level. 13.1.5 Statement whether or not leakage occurred and, if possible, a report of the location of each leak. 13.1.6 Statement of the number of specimens included in the test and the number of failures, if any. 13.1.7 Conditioning time, temperature, and relative humidity. 13.1.8 Temperature and relative humidity of the test area. 13.1.9 Time between application and removal of closures. 13.1.10 Compilation of measured torques. 13.1.11 If Test Method B is used, a statement of vacuum and duration. 13.1.12 Statement of observations that may lead to improvements. 14. Precision and Bias 14.1 No statement is made about either the precision or bias of this test method since the result merely states whether there is conformance to the criteria for success specied in the procedure. 15. Keywords 15.1 closure leakage; container leakage; leak; leakage; liquid leakage; vacuum

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