1、Designation: D 3094 00 (Reapproved 2005)Standard Test Method forSeepage Rate of Aerosol Products1This standard is issued under the fixed designation D 3094; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision.
2、 A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the determination of approxi-mate mass loss due to valve seepage rate2of aerosol productsby the collection
3、and measurement of gases seeping throughthe valve and into a special eudiometer tube, over a relativelyshort time period.1.2 It can be shown that the average refrigeration-filledaerosol product seeps to the extent of approximately 3.0 mLwhen the corresponding mass loss is 0.10 oz (2.9 cm3)/year.This
4、 figure is partially based on air content and is subject tovariations according to filling conditions. This test method isnot considered dependable when applied to pressure-filled,unpurged aerosol products.1.3 This standard does not purport to address all of thesafety concerns, if any, associated wi
5、th its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Significance and Use2.1 This test method affords a more rapid answer to theever-present problem of mass lo
6、ss during storage. It is ofparticular value in determining the effectiveness of valve stakeand clinch seal elastomers in contact with new formulations.This test method may also be used to evaluate new valves withstandard mixtures.3. Apparatus3.1 Bath, constant-temperature, equipped with a thermo-reg
7、ulator sufficient to maintain water at 80 6 2F (26 6 1C).The tank should be of sufficient proportions to accommodatethe necessary number of test specimens in an upright position,so that each specimen is surrounded by approximately 1 in. (25mm) of water.3.2 Eudiometer Tubes (Fig. 1 and Fig. 2), custo
8、m-orderedor hand-made, with an internal volume of 5.0 mL net (allowingfor any part of the valve that might protrude into the tube). Itis convenient to calibrate in 1, 2, and 3-mL divisions.NOTE 1For tests involving many dispensers, small test tubes and vialshave been successfully substituted for the
9、 tubes in Fig. 1 and Fig. 2.4. Test Specimens4.1 Test specimens shall be prepared in accordance withproduction methods wherever possible, making certain that theclinch diameter and the depth of clinch below the curl of themounting cup are in agreement with the specifications. New1This test method is
10、 under the jurisdiction of ASTM Committee D10 onPackaging and is the direct responsibility of Subcommittee D10.33 on MechanicalDispensers. This test method was originally developed by the Chemical SpecialtiesManufacturers Assn.Current edition approved Oct. 1, 2005. Published October 2005. Originally
11、approved in 1972. Last previous edition approved in 2000 as D 3094 00.2Data on the theoretical development of seepage concepts has been filed atASTM Headquarters as RR:D-10-1000.NOTE 1The dimensions are approximate, and subject to the geometryof the valve.FIG. 1 Suggested Tube for Evaluation of Valv
12、e and Staked SealsNOTE 1The dimensions are approximate, and subject to the geometryof the valve.FIG. 2 Suggested Tube for Evaluation of Valve, and Staked andClinched Seals1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.dispensers sha
13、ll be pretested for leakage by heating thecontents to 130F (54C).5. Procedure5.1 Fill the bath with water that has been allowed todeaerate for 24 h at room temperature. Bring the bath to 80F(26C) and immerse the dispensers.5.2 Scrub the bath walls, bottom, and dispenser surfaces toremove adhering ai
14、r. Give the dispensers a hard knock torelease any air bubbles clinging to the valve parts.5.3 Submerge the eudiometer tubes and fill them. Removethe air bubbles. Invert the tubes over the dispenser valves andallow them to remain for 48 h.5.4 Give each dispenser a hard knock to free the clinginggas i
15、nto the inverted eudiometer tube. Determine and recordthe amount of gas in each tube.5.5 The mass loss due to seepage through the valve andO-ring seal represents only a part of the total mass loss.Leakage will also occur at the seams and seam junctures.5.6 There is usuallya1to2-week adjustment perio
16、d withnew dispensers, during which some perturbations in seepagerate will occur. After this, a reasonably steady day-to-day rateis assumed.NOTE 2Many dispensers are found to rust slightly when stored underwater for 2 days. This condition may be remedied by employing a bathsolution containing 0.5 % s
17、odium nitrate (NaNO3) and 0.5 % triethyleneglycol in water. In a more concentrated solution, triethylene glycol exertsa softening effect upon enamel dispenser finishes.6. Calculation6.1 Correct the volume of gas collected in the eudiometertube to allow for water solubility. Since the degree of solub
18、ilitydiffers with the composition of gas, use the following equationsin accordance with the chemical content of freshly diffusedgas:For all mixtures of P-11 and P-12:Vc5 Vo5 0.29 1 0.66 NP 5 11! (1)For difluorodichloromethane only:Vc5 Vo1 0.29 (2)For trichlorofluoromethane only:Vc5 Vo1 0.95 (3)where
19、:Vc= corrected column of gases in eudiometer tube,Vo= 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 thetube (before selective solubility changes the gascomposition).NOTE 3Eq 2 and Eq 3 are special case
20、s of Eq 1. Eq 1 is simplified andaccurate to 0.1 mL only.6.2 Corrections for aerosols containing several standardpropellants are presented in Fig. 3. All data is based on the useof standard 5.0-mL eudiometer tubes. For example, an air-freeaerosol containing 50 % each of P-11 and P-12 as propellantsw
21、ill diffuse an observed 2.73 mL of gas under test conditionswhen the seepage is 0.10 oz (2.9 cm3)/year through the valve.The gas will be predominantly difluorodichloromethane.7. Precision and Bias7.1 Precision The precision of D 3094 is highly depen-dent on the contents and type of aerosol packaging
22、 beingtested. One laboratory conducted a seepage test on a water-based hair mousse. The results are shown in Table 1. Theresults of this test are dependent on variations in filling thecontents (both propellant and product concentrate), the solu-bility of the propellant used, the head space in the pa
23、rticularcan as well as the level of the product in the can at the time oftesting.7.2 BiasTest Method D 3094 has no bias because anaccepted reference or referee value is not available.Aerosol Liquid Phase Composition: 50 % P-11 + 50 % P-12 67%P-12+33%P-11_100 % P-12FIG. 3 Fate of Gases Seeping Throug
24、h Aerosols and into a5.0-mL Eudiometer Tube Filled with WaterTABLE 1 Results of Seepage TestABubble Size Actual PropellentLossNo. of Units Estimated AnnualWeight Loss4mL 7.12mL 1 2.53g5mL 8.12mL 4 2.88g6mL 9.12mL 5 3.24g7 mL 10.12 mL 2 3.59 gAActual propellent loss is Bubble Size + Soluble Gases.Sol
25、uble Gases = 0.13 mL/mL of Water 3 24 mL tube = 3.12 mL soluble gases.D 3094 00 (2005)2ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of
26、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 must be reviewed every five years andif not revised, either reapproved or withdrawn. Y
27、our 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 theresponsible technical committee, which you may attend. If you feel that your commen
28、ts 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, 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).D 3094 00 (2005)3
