Designation D5094/D5094M − 09 (Reapproved 2014) Standard Test Methods for Gross Leakage of Liquids from Containers with Threaded or Lug Style Closures1 This standard is issued under the fixed designat[.]
Designation: D5094/D5094M − 09 (Reapproved 2014) Standard Test Methods for Gross Leakage of Liquids from Containers with Threaded or Lug-Style Closures1 This standard is issued under the fixed designation D5094/D5094M; 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 Scope D996 Terminology of Packaging and Distribution Environments D999 Test Methods for Vibration Testing of Shipping Containers D3198 Test Method for Application and Removal Torque of Threaded or Lug-Style Closures D3474 Practice for Calibration and Use of Torque Meters Used in Packaging Applications D4169 Practice for Performance Testing of Shipping Containers and Systems D4332 Practice for Conditioning Containers, Packages, or Packaging Components for Testing D7386 Practice for Performance Testing of Packages for Single Parcel Delivery Systems 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 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 Terminology 3.1 General definitions for packaging are found in Terminology D996 3.2 Definitions of Terms Specific to This Standard: 3.2.1 gross leak—any 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 leak—any opening in a container which, contrary to intention, either lets contents escape or permits substances to enter 3.2.3 leakage—that which passes through a leak 1.3 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 1.4 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 Summary of Test Methods 4.1 Method A, Shipping Container Vibration and Storage Test—Test specimens are filled to their expected fill 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 40°C [104°F] (or other conditions as appropriate) for four weeks Each specimen is examined for leakage Referenced Documents 2.1 ASTM Standards:2 This test method is under the jurisdiction of ASTM Committee D10 on Packaging and is the direct responsibility of Subcommittee D10.32 on Consumer, Pharmaceutical, Medical, and Child Resistant Packaging Current edition approved Oct 1, 2014 Published November 2014 Originally approved in 1990 Last previous edition approved in 2009 as D5094/D5094M – 09 DOI: 10.1520/D5094_D5094M-09R14 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 standard’s Document Summary page on the ASTM website 4.2 Method B, Container Vibration and Vacuum Chamber Test—Test specimens are partially filled 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 Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959 United States D5094/D5094M − 09 (2014) 7.3 Select unused closures and unused containers that are within specifications 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 –34 kPa [10 in Hg] vacuum for 10 and examined for leakage Test Specimens 8.1 Test Method A—A specimen shall be one container filled to expected fill capacity with product or liquid simulating product The closure is secured in accordance with 11.1 NOTE 1—Other levels of vacuum, or time, or both may be appropriate Significance and Use 8.2 Test Method B—A specimen shall be one container one-third filled with product or liquid simulating product The closure is secured in accordance with 11.1 5.1 These test methods are used to indicate the integrity of the container and closure system in the distribution environment 8.3 Colorant should be added to the contents when necessary to give permanent indication where there is leakage 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 Calibration 9.1 Calibrate the torque meter in accordance with Practice D3474 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 10 Conditioning 10.1 Store the shipping container components at ambient laboratory conditions for at least h before testing, or other conditions in accordance with Practice D4332 Apparatus 10.2 Store the torqued container/closure test specimens upright at least 24 h at ambient conditions before commencing the test 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 1°C [104 1.8°F] 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 Test Methods D999 may be used 11 Procedure 11.1 Apply closures to the containers according to the Application Torque Measurement section of the procedure in Test Method D3198 11.2 Test Method A, Shipping Container Vibration and Storage Test: 11.2.1 Place the filled specimens in their shipping container or in an appropriate carton so that they will remain firmly in place during vibration 11.2.2 Proceed as directed according to Test Methods D999 (Method A1 or A2) 20 each on bottom, top, and one side, or run an entire shipping cycle in accordance with Practice D4169 (for multiple parcel shipments) or with Practice D7386 (for single parcel shipments) 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 finish/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° 1°C [104° 1.8°F], or other appropriate temperature, ambient humidity (see the Preferred Atmospheres listing in Practice D4332) 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 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, fitted 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 to –100 kPa [0 to 30 in Hg] 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 Test Methods D999 may be used 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 fill the shipping container More than one shipping container may be required 11.3 Test Method B, Shipping Container Vibration and Vacuum Chamber Test: D5094/D5094M − 09 (2014) 13 Report 11.3.1 Place the partially filled specimens in their shipping container or in an appropriate carton so that they will remain firmly in place during vibration 11.3.2 Proceed as directed according to Test Methods D999 (Method A1 or A2) 20 each on bottom, top, and one side, or run an entire shipping cycle in accordance with Practice D4169 (for multiple parcel shipments) or with Practice D7386 (for single parcel shipments) as desired 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 filled specimens inverted in a beaker or other receptable to contain leakage 13.1 Report the following information: 13.1.1 Statement that testing was done in accordance with ASTM Test Method D5094, Test Method A or Test Method B, or that the testing was done with indicated changes 13.1.2 Description of shipping cycle(s) used: per Practice D4169 or Practice D7386, or both 13.1.3 Materials of construction of the closure, liner and container including finish and manufacturer’s designation 13.1.4 Description of the shipping container and interior packaging, the test frequencies, intensities, and durations used 13.1.5 Product or substitute used and fill level 13.1.6 Statement whether or not leakage occurred and, if possible, a report of the location of each leak 13.1.7 Statement of the number of specimens included in the test and the number of failures, if any 13.1.8 Conditioning time, temperature, and relative humidity 13.1.9 Temperature and relative humidity of the test area 13.1.10 Time between application and removal of closures 13.1.11 Compilation of measured torques 13.1.12 If Test Method B is used, a statement of vacuum and duration 13.1.13 Statement of observations that may lead to improvements NOTE 2—Other orientations of the specimens may be appropriate 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 min) to –34 kPa [10 in Hg] and close the outlet valve 11.3.8 Maintain the vacuum for 10 11.3.9 Partially open the chamber inlet valve and release the vacuum slowly (30 s to 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 14 Precision and Bias 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 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 specified in the procedure 15 Keywords 15.1 closure leakage; container leakage; leak; leakage; liquid leakage; vacuum 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 This 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