1、Designation: D 3090 72 (Reapproved 2003)Standard Practice forStorage Testing of Aerosol Products1This standard is issued under the fixed designation D 3090; 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.This standard has been approved for use by agencies of the Department of Defense.1. Scope1.1 This practice covers the storage testing of aeroso
3、lproducts.1.2 There are two major types of storage tests that may beperformed on aerosol products:1.2.1 Live Storage Tests, where the valves are actuated andthe determinations are made at relatively frequent intervals (thepurpose being to simulate consumer use of aerosol dispensers),and1.2.2 Dead St
4、orage Tests, performed to simulate warehousestorage conditions when shelf-life information is sought.1.3 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and hea
5、lth practices and determine the applica-bility of regulatory limitations prior to use. For specificprecautionary statements, see Section 4.2. Significance and Use2.1 Aerosol products are subjected to storage tests to ascer-tain the shelf-life of the complete package, and to evaluate thedegree of sui
6、tability of the valve and container components fortheir intended uses.2.2 It is impractical to promulgate a standard procedure forconducting storage tests, since variations will be necessitatedby differences in the ultimate objective (for example, theprimary interest of one test may be concerned wit
7、h containersuitability or shelf-life of a new product in an existing package,while another test may be concerned with valve evaluation).2.3 It follows that storage testing must be flexible enough toaccommodate the small procedural changes required. Thus,this recommended practice will only set forth
8、those principlesto be observed in establishing a definite procedure, in order toallow the individual operator the prerogative of adapting theseto satisfy his particular requirements.3. General Requirements3.1 Before making any aerosol storage tests, the followingshould be borne in mind:3.1.1 Suffici
9、ent test specimens should be available to re-place any that fail during the test, and to make it possible toextend the storage period if desired.3.1.2 The test schedule and procedure should be wellplanned. Only if this is followed, can there be any assurancethat important developments have not been
10、missed, and that theresults will correlate with other storage test results.3.1.3 The tests should be performed by competent personnelwell qualified in the field. Since most of the data is not obtainedby direct measurement and is therefore not entirely objective innature, it is highly desirable to ha
11、ve the same operator performall of the tests on a given specimen. This, in addition to 3.1.2,will do much to minimize the effect of the human element.3.2 Before any specimens are committed to storage, thefollowing should apply:3.2.1 All pertinent background information concerning theproblem should b
12、e assembled, so that the test specimen can beintelligently set up.3.2.2 Tests should be conducted to eliminate defectivecontainers and valves (the frequency of such defects should berecorded). To make this segregation possible, pressure deter-minations, hot bath, vial leakage, and spray tests should
13、 bemade on each filled dispenser.3.2.3 Conditions of filling and handling should as closely aspossible approximate those that would be encountered com-mercially.4. Safety Precautions4.1 Aerosol storage tests involve a container, valve, orproduct of unknown compatibility and performance. For thisreas
14、on, serious accidents could occur. The operator shouldemploy gloves, safety shield, safety glasses, and apparatus withproper controls.4.2 If, during a test, container perforations or signs ofadvanced corrosion are found, or if the product, dispensers, orvalves otherwise become unmerchantable, the en
15、tire lot of1This practice is under the jurisdiction of ASTM Committee D10 on Packagingand is the direct responsibility of Subcommittee D10.33 on Mechanical Dispensers.This practice was originally developed by the Chemical Specialties ManufacturersAssociation.Current edition approved July 28, 1972. P
16、ublished November 1972.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.specimens should be destroyed. Continued testing would wastetime and space, and could result in a serious accident.5. Live Storage Test5.1 Test TemperatureSpecime
17、ns should be stored at roomtemperature. In addition, a higher-temperature storage (forexample, 98F (36C) may be employed. The use of thehigher-temperature storage is particularly desirable when anew valve or product is being evaluated. The use of storagetemperatures below 32F (6 0C), or the alternat
18、e exposure tosubfreezing and elevated temperatures, has considerable meritin the screening of new valves or new valve materials.5.2 Test Position and Number of SpecimensIf the purposeof the test is to evaluate a valve, half of the specimens at eachstorage temperature should be kept in an inverted po
19、sition. Ifthe product, or any constituent thereof, exerts a detrimentaleffect on the sealing material of the valve, the conditions maybe more readily observed in the case of inverted cans. Six cansinverted and six cans upright for each temperature is theminimum number of specimens for each variable
20、that shouldbe considered. If the test involves only one temperature, ten totwelve cans per variable (upright and inverted) is a moredesirable size.5.3 Test TimeThe tests are usually considered completedwhen 10 g or less of formulation remains in the containers.Extension of the tests beyond this poin
21、t may cause erratic andunreliable results.5.4 Examination ScheduleExaminations of the specimensshould be made weekly, or more often if the completion of thetest in less total elapsed time is necessary.5.5 FailureIf a valve becomes totally inoperative or failsto operate properly, the container and va
22、lve should be imme-diately torn down to ascertain the cause of failure.5.6 Final ExaminationEach container and valve shouldbe critically examined as soon as possible after the final valveactuation of the test.6. Dead Storage Test6.1 Test Temperature:6.1.1 Specimens are usually stored at 98F (36C) an
23、d roomtemperature, while other temperatures are employed in specialcases.6.1.2 Temperatures from 95 to 100F (35 to 37C) (oftenreferred to as incubation temperature) may accelerate containercorrosion and leakage, if the containers are so predisposed.However, incubated storage should always be used in
24、 conjunc-tion with room temperature since it is often difficult, if notimpossible, to predict a normal shelf-life on the basis of 98Ftests alone.6.1.3 Storage below freezing (0 to 32F (17 to 0C) isvaluable for evaluating the sealing efficiency and suitability ofthe gasket materials in aerosol valves
25、.6.1.4 Storage at 130F (54C) should be employed when theresistance of the container to structural fatigue is to bedetermined.6.2 Test Position and Number of Specimens:6.2.1 Specimens at each storage temperature should be heldin both upright and inverted positions.6.2.2 Enough specimens should be pro
26、vided for each test sothat a minimum of two dispensers of each variable from eachtemperature can be evaluated and torn down at each scheduledexamination. The other specimens remain untouched, with theexception of weighing, until they are needed at a subsequentexamination.6.2.3 A minimum of twelve ex
27、tra specimens per variableshould be stored at each temperature to allow for extension ofthe test, if this later becomes necessary, and to allow a largernumber of specimens to be inspected at the final examination.6.2.4 Thus, the minimum suggested number of specimensper product, container, or valve v
28、ariable is as follows:4np4 1 y! (1)where:y = duration of the test, years,n = number of storage temperatures, andp = number of storage positions to be employed.6.2.5 It is usually desirable to include a glass bottle of theaerosol concentrate with the specimens, in order to determinedeteriorations tha
29、t may take place that are independent of theaerosol container. One or two glass aerosol containers may alsobe included.6.2.6 It is often useful to place one or two empty metalcontainers with the specimens, especially for internally linedvariables, for possible future references.6.3 Test TimeMost dea
30、d storage tests are concluded after24 months of storage, but a test may be extended for a muchlonger period, if the previous results and the objective sorequire.6.4 Examination ScheduleExaminations are usually madeat 1, 3, and 6-month intervals, and at 6-month intervalsthereafter, until the test is
31、completed.7. Examination7.1 The examination of the specimen may be divided intoperformance determination, container and valve inspection,and product evaluation.7.2 The performance of the complete specimen may beascertained by making mass loss, discharge rate (10 s),pressure, and possibly particle si
32、ze determinations. At eachexamination, the mass loss and discharge rate should bemeasured. Internal pressure determinations at each examina-tion are usually not necessary, but it is recommended that thepressures be taken initially and two or three equally spacedtimes during the test.7.3 As a check o
33、n filling, the volatile-nonvolatile ratio maybe determined following the examinations.7.4 After expulsion of the propellant, the product should betransferred and the container and valve carefully torn down andexamined. The metal valve parts should be carefully inspectedfor evidences of corrosion, an
34、d the rubber or plastic compo-nents should be checked for swelling, softening, or disintegra-tion. Conditions in the container interiors should then be notedwith special emphasis on any staining, detinning, rusting,pitting, or other indications of corrosion that may be present.Microscopical examinat
35、ion of the valve and container compo-nents is recommended, for without this assistance importantand indicative developments may be overlooked.D 3090 72 (2003)27.5 The product from the containers should be examined forcolor change and precipitate or sludge formation. If corrosionis found or suspected
36、 in the container, it is suggested that theproduct be analyzed for the moisture, iron, and tin content.7.6 If any abnormal or undesirable conditions are found inthe performance of the valve or product, sufficient additionalspecimens of the same lot should be examined to confirm thefindings.7.7 If en
37、tomological data are required, they may be obtainedby using pertinent existing standard procedures.7.8 See Table 1 for a sample aerosol product storage test(both dead and live storage).7.9 See Appendix X1 for other tests that may be run inconjunction with an aerosol storage testing program.8. Keywor
38、ds8.1 aerosol products; aerosol products storage; shelf-life ofaerosol packaging; storage testing; storage testing aerosolproductsAPPENDIX(Nonmandatory Information)X1. OTHER RECOMMENDED TESTSX1.1 There are several other tests that should be consideredin conjunction with an aerosol storage testing pr
39、ogram.X1.2 In evaluating a valve for a given formulation, it maybe desirable to subject the containers to a continuous dischargetest, whereby the containers are emptied in a single burst or aseries of long bursts. This procedure is very rapid, and maygive valuable clues on the suitability of the val
40、ve gasketmaterial for the product. If indications of weakening, disinte-gration, or undue swelling of the valve gaskets are found bymeans of this test, particular attention should be directed to theresults of the live storage test.X1.3 Before commercial packaging of a new product or theuse of a new
41、container or valve is approved, it is desirable toobtain certain information outside the scope of the laboratorytest:X1.3.1 Filled containers should be subjected to normalhandling, cartoning, and shipping operations to determine thesuitability of protective devices and the resistance of thecontainer
42、s and valves to shock.X1.3.2 Containers should be shipped to and stored inwarehouses having the extremes in temperatures that could beencountered in the distribution and marketing of the product.After a predetermined storage period in the various locations,the containers should be returned to the la
43、boratory for acomplete examination.X1.4 Once commercial packaging of a product is initiated,a program may be inaugurated whereby defective or complaintdispensers encountered in the field are returned to the labora-tory. By this means, a continuous check on the quality ismaintained, and it may enable
44、 the manufacturer and packer tobe forwarned of any difficulty before it becomes serious, sothat corrective measures may be taken.TABLE 1 Sample Aerosol Product Storage TestLive Storage Dead StorageProduct, container; valve variables 2 (product) 2 (product)Storage temperatures room temperature, 98F (
45、36C) 30F (1C), room temperature, 98F (36C),130F (54C)Storage positions upright and inverted upright and invertedNumber of filled cans per formulation 24 (half inverted at each temperature) 144 (half inverted at each temperature)Total Number of filled cans 48 (half inverted) 288Duration of test until
46、 completed 2 yearsExamination schedule weekly 1, 3, 6, 12, 18, 24 monthsNo. of containers examined each examination 48 cans 24 cans (2 per product per temperature perposition), all remaining dispensers examined after24 months shortage (all dispensers weighed)Examination procedure mass loss mass loss
47、pressure pressuredischarge rate (10 s) discharge rate (10 s)(particle size) valve examinationvalve and container inspection container examination(at final examination or product examinationwhen failure occurs)D 3090 72 (2003)3ASTM International takes no position respecting the validity of any patent
48、 rights asserted in connection with any item mentionedin 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
49、 any time by the responsible technical committee and must 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 theresponsible 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 s
