1、Designation: D3094 00 (Reapproved 2010)D3094 18Standard Test Method Practice forSeepage Rate of Aerosol Products1This standard is issued under the fixed designation D3094; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of
2、 last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method practice covers the determination of approximate mass loss due to valve seepage rate2 of aerosol pro
3、ductsby the collection and measurement of gases seeping through the valve and into a special eudiometer tube, over a relatively shorttime period.1.2 It can be shown that the average refrigeration-filled aerosol product seeps to the extent of approximately 3.0 mL when thecorresponding mass loss is 0.
4、10 oz (2.9 cm3)/year. This figure is partially based on air content and is subject to variations accordingto filling conditions. This test method practice is not considered dependable when applied to pressure-filled, unpurged aerosolproducts.1.3 The values stated in inch-pound units are to be regard
5、ed as standard. The values given in parentheses are mathematicalconversions to SI units that are provided for information only and are not considered standard.1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the use
6、r of this standard to establish appropriate safety safety, health, and healthenvironmental practices and determine theapplicability of regulatory limitations prior to use.1.5 This international standard was developed in accordance with internationally recognized principles on standardizationestablis
7、hed in the Decision on Principles for the Development of International Standards, Guides and Recommendations issuedby the World Trade Organization Technical Barriers to Trade (TBT) Committee.2. Significance and Use2.1 This test method practice affords a more rapid answer to the ever-present problem
8、of mass loss during storage. It is ofparticular value in determining the effectiveness of valve stake and clinch seal elastomers in contact with new formulations. Thistest method practice may also be used to evaluate new valves with standard mixtures.3. Apparatus3.1 Bath, constant-temperature, equip
9、ped with a thermo-regulator sufficient to maintain water at 80 6 2F (26 6 1C). The tankshould be of sufficient proportions to accommodate the necessary number of test specimens in an upright position, so that eachspecimen is surrounded by approximately 1 in. (25 mm) of water.3.2 Eudiometer Tubes (Fi
10、g. 1 and Fig. 2), custom-ordered or hand-made, with an internal volume of 5.0 mL net (allowing forany part of the valve that might protrude into the tube). It is convenient to calibrate in 1, 2, and 3-mL divisions.NOTE 1For tests involving many dispensers, small test tubes and vials have been succes
11、sfully substituted for the tubes in Fig. 1 and Fig. 2.4. Test Specimens4.1 Test specimens shall be prepared in accordance with production methods wherever possible, making certain that the clinchdiameter and the depth of clinch below the curl of the mounting cup are in agreement with the specificati
12、ons. New dispensers shallbe pretested for leakage by heating the contents to 130F (54C).5. Procedure5.1 Fill the bath with water that has been allowed to deaerate for 24 h at room temperature. Bring the bath to 80F (26C) andimmerse the dispensers.1 This test method practice is under the jurisdiction
13、 of ASTM Committee D10 on Packaging and is the direct responsibility of Subcommittee D10.33 on MechanicalDispensersAerosol Products. This test method practice was originally developed by the Chemical Specialties Manufacturers Assn.Current edition approved Oct. 1, 2010May 1, 2018. Published November
14、2010June 2018. Originally approved in 1972. Last previous edition approved in 20052010 asD3094 00 (2005). (2010). DOI: 10.1520/D3094-00R10.10.1520/D3094-18.2 Data on the theoretical development of seepage concepts has been filed atASTM Headquarters as RR:D10-1000. ContactASTM Customer Service at ser
15、viceastm.org.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users cons
16、ult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States15.2 Scrub the bath walls, bottom, a
17、nd dispenser surfaces to remove adhering air. Give the dispensers a hard knock to releaseany air bubbles clinging to the valve parts.5.3 Submerge the eudiometer tubes and fill them. Remove the air bubbles. Invert the tubes over the dispenser valves and allowthem to remain for 48 h.5.4 Give each disp
18、enser a hard knock to free the clinging gas into the inverted eudiometer tube. Determine and record theamount of gas in each tube.5.5 The mass loss due to seepage through the valve and O-ring seal represents only a part of the total mass loss. Leakage willalso occur at the seams and seam junctures.5
19、.6 There is usually a 1 to 2-week adjustment period with new dispensers, during which some perturbations in seepage rate willoccur. After this, a reasonably steady day-to-day rate is assumed.NOTE 2Many dispensers are found to rust slightly when stored under water for 2 days. This condition may be re
20、medied by employing a bath solutioncontaining 0.5 % sodium nitrate (NaNO3) and 0.5 % triethylene glycol in water. In a more concentrated solution, triethylene glycol exerts a softeningeffect upon enamel dispenser finishes.6. Calculation6.1 Correct the volume of gas collected in the eudiometer tube t
21、o allow for water solubility. Since the degree of solubility differswith the composition of gas, use the following equations in accordance with the chemical content of freshly diffused gas:For all mixtures of P-11 and P-12:Vc 5Vo 50.2910.66 NP511! (1)For difluorodichloromethane only:Vc 5Vo10.29 (2)F
22、or trichlorofluoromethane only:Vc 5Vo10.95 (3)where:Vc = corrected column of gases in eudiometer tube,NOTE 1The dimensions are approximate, and subject to the geometry of the valve.FIG. 1 Suggested Tube for Evaluation of Valve and Staked SealsNOTE 1The dimensions are approximate, and subject to the
23、geometry of the valve.FIG. 2 Suggested Tube for Evaluation of Valve, and Staked and Clinched SealsD3094 182Vo = observed volume of gases in eudiometer tube, andNP = 11 = mole fraction or volume %/100 of trichloro- fluoromethane in the gas as it is diffused into the tube (before selectivesolubility c
24、hanges the gas composition).NOTE 3Eq 2 and Eq 3 are special cases of Eq 1. Eq 1 is simplified and accurate to 0.1 mL only.6.2 Corrections for aerosols containing several standard propellants are presented in Fig. 3. All data is based on the use ofstandard 5.0-mL eudiometer tubes. For example, an air
25、-free aerosol containing 50 % each of P-11 and P-12 as propellants willdiffuse an observed 2.73 mL of gas under test conditions when the seepage is 0.10 oz (2.9 cm3)/year through the valve. The gaswill be predominantly difluorodichloromethane.7. Precision and Bias7.1 PrecisionThe precision of D3094
26、is highly dependent on the contents and type of aerosol packaging being tested. Onelaboratory conducted a seepage test on a water-based hair mousse. The results are shown in Table 1. The results of this test aredependent on variations in filling the contents (both propellant and product concentrate)
27、, the solubility of the propellant used, thehead space in the particular can as well as the level of the product in the can at the time of testing.7.2 BiasTest Method Practice D3094 has no bias because an accepted reference or referee value is not available.Aerosol Liquid Phase Composition: 50 % P-1
28、1 + 50 % P-12 67 % P-12 + 33 % P-11_ 100 % P-12FIG. 3 Fate of Gases Seeping Through Aerosols and into a 5.0-mL Eudiometer Tube Filled with WaterTABLE 1 Results of Seepage TestABubble Size Actual PropellentLossNo. of Units Estimated AnnualWeight Loss4 mL 7.12 mL 1 2.53 g5 mL 8.12 mL 4 2.88 g6 mL 9.12
29、 mL 5 3.24 g7 mL 10.12 mL 2 3.59 gA Actual propellent loss is Bubble Size + Soluble Gases.Soluble Gases = 0.13 mL/mL of Water 24 mL tube = 3.12 mL soluble gases.D3094 183ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin
30、 this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and mus
31、t be reviewed every five years andif not revised, either reapproved or withdrawn.Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of ther
32、esponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake 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,
33、 West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http:/ 184
