ASTM D4991 - 25 用真空法进行空刚性容器泄漏测试的标准试验方法

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Designation: D4991 −25

Standard Test Method for

Leakage Testing of Empty Rigid Containers by Vacuum

Method

This standard is issued under the ﬁxed designation D4991; 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

1.1 This test method covers the testing of empty containers

for resistance to leakage under differential pressure conditions

such as those which can occur during air transport. It is suitable

for testing rigid containers intended for the transportation of

some hazardous liquids in accordance with the United Nations

Recommendations On The Transport Of Dangerous Goods

(UN TDG) and the International Civil Aviation Organization

Technical Instructions For The Safe Transport Of Dangerous

Goods By Air (ICAO TIs).

1.2 This standard does not purport to address all of the

safety concerns, if any, associated with its use. It is the

responsibility of the user of this standard to establish appro-

priate safety, health, and environmental practices and deter-

mine the applicability of regulatory limitations prior to use.

1.3 This international standard was developed in accor-

dance with internationally recognized principles on standard-

ization established in the Decision on Principles for the

Development of International Standards, Guides and Recom-

mendations issued by the World Trade Organization Technical

Barriers to Trade (TBT) Committee.

2. Referenced Documents

2.1 ASTM Standards:

D996 Terminology of Packaging and Distribution Environ-

ments

D3078 Test Method for Determination of Leaks in Flexible

Packaging by Bubble Emission

2.2 United Nations Document:

ST/SG/AC.10/1 Recommendations On The Transport Of

Dangerous Goods

2.3 International Civil Aviation Organization:

DOC 9284-AN/905 Technical Instructions For The Safe

Transport Of Dangerous Goods By Air

3. Terminology

3.1 Deﬁnitions: Terms and deﬁnitions used in this test

method may be found in Terminology D996.

3.2 Deﬁnitions of Terms Speciﬁc to This Standard:

3.2.1 rigid container—a container sufficiently rigid that

under a positive pressure of 100 kPa gauge the volumetric

expansion does not exceed 0.5 %, such as a glass bottle.

4. Summary of Test Method

4.1 An empty rigid container to be tested is pressurized by

immersion in an ethylene glycol-water solution in a transparent

test chamber and subjected to a gradually increasing partial

vacuum. The container is observed for signs of leakage, as

evidenced by escaping air bubbles during depressurization or

ﬂuid in the container after re-pressurization.

5. Signiﬁcance and Use

5.1 Containers may be pressurized in accordance with this

test method without modiﬁcation to the closure or to the body

of the container. This test method may be used for testing rigid

containers intended for the transportation of some liquids by air

in accordance with the ICAO TIs or in accordance with the UN

TDG.

5.2 This test method establishes the point at which leakage

commences, with a limit of approximately 95 kPa (13.8 psi)

differential. See Test Method D3078 for ﬂexible packages.

5.3 This test method may not be suitable for some packages,

such as packages with paper cap seals, where the test ﬂuid may

rapidly deteriorate the packaging.

6. Apparatus

6.1 Transparent Vessel, large enough to permit the test

specimen(s) to be immersed in the test ﬂuid with a minimum

This test method is under the jurisdiction of ASTM Committee D10 on

Packaging and is the direct responsibility of Subcommittee D10.21 on Shipping

Containers and Systems - Application of Performance Test Methods.

Current edition approved Oct. 1, 2025. Published November 2025. Originally

approved in 1994. Last previous edition approved in 2023 as D4991 – 07 (2023).

DOI: 10.1520/D4991-25.

For referenced ASTM standards, visit the ASTM website, www.astm.org, or

contact ASTM Customer Service at www.astm.org/contact. For Annual Book of

ASTM Standards volume information, refer to the standard’s Document Summary

page on the ASTM website.

Available from United Nations Sales Section, United Nations, New York, NY

10017.

Available from Intereg Group, Inc., 5724 N. Pulaski Rd., Chicago, IL 60646.

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.

headspace of 20 %, capable of withstanding at least 1

⁄

-atm

pressure differential, ﬁtted with a ﬂat vacuum-tight cover is

required.

6.2 Vacuum Gauge, Inlet Tube from a Source of Vacuum,

and Outlet Tube to the Atmosphere, shall be sealed into the

cover. The inlet and outlet tubes shall be equipped with

handoperated valves. The vacuum gauge shall be laboratory

quality with a full-scale range from 0 kPa to 100 kPa (0 psi to

14.5 psi) with minimum graduations no greater than 2 kPa

(0.3 psi) and accuracy to within 1 %. A suitable moisture trap,

to prevent back-ﬂow of liquid, should be ﬁtted between the

vacuum gauge and the source of vacuum.

6.3 Solution of Ethylene Glycol in Water, 50 % by Volume

for use as a test ﬂuid, at ambient temperature unless otherwise

speciﬁed, is required. Where a test temperature other than

ambient is speciﬁed, the solution shall be at the speciﬁed test

temperature. Other solutions may be required for high and low

temperatures.

NOTE 1—If ethylene glycol antifreeze solution is used, it should be

clariﬁed by ﬁltering through activated charcoal.

6.4 A suitable means to hold the test specimen(s) with the

closure(s) not less than 25 mm (1 in.) under the surface of the

test ﬂuid is required. The method of restraint should not affect

the results of the test.

7. Test Specimens

7.1 Test specimens shall consist of containers, including

their closures. Test specimens of containers which are in

production shall be representative samples, taken at random.

7.2 Containers shall be empty containers which previously

contained any substance and were cleaned of the contents prior

to testing. New containers and closures, where available,

should be used.

7.3 Each container shall be closed for testing in the same

manner as it would be closed for actual shipment. All closures

shall be installed using the techniques or torques speciﬁed by

the closure manufacturer, container manufacturer, or shipper.

Close containers at ambient pressure and temperature.

7.4 Where a test temperature other than ambient is speciﬁed,

the sample containers shall be conditioned at the test tempera-

ture for at least 24 h, and until they reach equilibrium of

temperature with the conditioning atmosphere.

7.5 Unless otherwise speciﬁed, test at least three specimens.

8. Preparation of Apparatus

8.1 Assemble the apparatus in accordance with Fig. 1.

8.2 Prior to testing, draw a vacuum to at least 95 kPa

(13.8 psi) differential and maintain this vacuum for 10 min in

order to remove air dissolved in the test ﬂuid.

9. Procedure

9.1 Immerse the test specimens in the ethylene glycol-water

solution inside the transparent test chamber. Remove as many

bubbles as possible from the outer surface of the test specimens

by agitation or other means.

9.1.1 More than one specimen can be tested at one time

provided that there is sufficient space in the test chamber to

allow clear observation of each specimen. If this is done, affix

the test specimens so closures are sufficiently separated to

permit individual observation of each, to detect leakage.

9.2 Seal the lid, open the hand valve on the inlet tube, and

close the hand valve on the outlet tube to the atmosphere. Turn

on the vacuum so that the gauge rises slowly (from 30 s to

1 min) to a pressure differential of 95 kPa (13.8 psi), or other

speciﬁed pressure differential. The vacuum can be controlled

by cracking open the hand valve on the outlet tube. During the

rise in vacuum, observe the test specimen(s) for leakage as

evidenced by a continuous stream or recurring succession of

small bubbles. Isolated bubbles caused by trapped air are not

considered evidence of leakage. Maintain the vacuum for a

minimum of 10 min. For test specimens which are single

packagings or combination packagings in whole or part of

plastic material, maintain the vacuum for 30 min. Then turn the

vacuum off and release it slowly by opening the hand valve on

the outlet tube. Keep the test specimen(s) immersed for at least

30 s at ambient pressure. Remove the test specimen(s) and

examine the inside for ﬂuid.

9.3 Leakage is indicated by a continuous stream or recurring

succession of bubbles. Fluid within the test specimen is also

evidence of leakage.

10. Report

10.1 Report the following information:

10.1.1 Identiﬁcation of the containers and closures, using

manufacturer’s part numbers and descriptions or using ex-

ploded view drawings or cross-sectional drawings, including

detailed data on material construction,

10.1.2 Total number of specimens tested,

10.1.3 Number of specimens tested at one time,

10.1.4 Test pressure requirement, where applicable,

10.1.5 Whether test was performed at ambient temperature

and if not, the test temperature. If a test solution other than

50 % ethylene glycol was used, identify the solution,

10.1.6 Whether test specimens passed or failed the test,

where applicable,

10.1.7 Whether each test specimen leaked and at what

pressure differential,

FIG. 1 Typical Test Setup for Leakage Testing of Containers by

Vacuum Method

D4991 − 25

10.1.8 Whether test ﬂuid was apparent in each test specimen

after testing,

10.1.9 A statement to the effect that all tests were made in

full compliance with the requirements of this test method, or

noting any variations and detailing them, and

10.1.10 The name and address of the testing agency, the

date, and the signature of a responsible representative of the

testing agency.

11. Precision and Bias

11.1 No information is presented about either the precision

or bias of this test method for measuring leaking of rigid plastic

containers since the result is non-quantitative. It is recom-

mended that test sensitivities be determined and a positive and

negative control be used when validating the test method.

11.2 Once validated, the user does not have to apply the

positive and negative controls before each test.

12. Keywords

12.1 containers; leakage testing; packaging; vacuum

method

APPENDIX

(Nonmandatory Information)

X1. TABLE X1.1

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

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 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), or through the ASTM website (www.astm.org/contact). Permission rights to photocopy the

standard may also be secured from the Copyright Clearance Center, 222 Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600;

http://www.copyright.com/

TABLE X1.1 Pressure Conversion Table—Pressure

Differential

KiloPascals Pounds per square

inch (psi)

Inches of mercury

in Hg (20 °C) Bar

10 1.45 2.96 0.10

20 2.90 5.93 0.20

30 4.35 8.89 0.30

40 5.80 11.85 0.40

50 7.25 14.82 0.50

60 8.70 17.78 0.60

70 10.15 20.75 0.70

75 10.88 22.23 0.75

80 11.60 23.71 0.80

85 12.33 25.19 0.85

90 13.05 26.67 0.90

95 13.78 28.16 0.95

100 14.50 29.64 1.00

101.325 14.70 30.03 1.01325

psi × 6.894757 = kPa

in. Hg × 3.37411 = kPa

bar × 100 = kPa

D4991 − 25

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标签： #标准试验 #试验方法 #标准试验方法

摘要：

ASTM D4991-25是权威的包装测试标准，规定了采用真空法对空刚性容器进行泄漏测试的标准试验方法。该方法通过将空容器置于受控真空环境中，依据内外压差变化或真空保持情况判断容器是否存在泄漏通道，适用于玻璃瓶、金属罐、塑料瓶等各类空刚性容器的密封性验证。标准内容涵盖测试仪器、样品准备、试验步骤、结果判定及报告要求，帮助生产企业有效识别因瓶口缺陷、瓶身裂纹、封装不良或材料薄弱等问题导致的泄漏风险。在药品、食品、日化、化工及运输包装等领域，ASTM D4991-25常被用于产品质量控制、生产线抽检

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