1、Designation: D 6654 05Standard Test Method forBasic Storage Stability of a Mechanical Pump Dispenser1This standard is issued under the fixed designation D 6654; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revis
2、ion. 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 the basicstorage stability of a mechanical pump dispenser with aproduct.1.2 This t
3、est method covers an evaluation of the weight lostduring storage of mechanical pump dispensers (spray or flowtypes) with a product.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 establi
4、sh appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 2063 Test Methods for Measurement of Torque Retentionfor Packages with Continuous Thread ClosuresD 3890 Test Method for Number of Strokes t
5、o Prime aMechanical Pump DispenserD 4336 Test Methods for Determination of Output perStroke of a Mechanical Pump DispenserE 122 Practice for Calculating Sample Size to Estimate,With a Specified Tolerable Error, the Average for aCharacteristic or Process3. Significance and Use3.1 Determining the stor
6、age of a mechanical pump dis-penser for consumer usage. Products of consumer usage are ofthe personal care, household, insecticides, food, automotive,and institutional nature. Pharmaceutical and cosmetic productsincluding perfume are not covered under this practice.4. Apparatus4.1 Containers, that w
7、ill allow the mechanical pump dis-penser to be affixed to them (see Note 1) and also be capableof containing product for a period of time at various environ-mental conditions (see Note 2).NOTE 1If possible, the actual container to be marketed should beused.4.2 Product, a sufficient amount to fill th
8、e number ofcontainers in accordance with 4.1, reference 10.2.4.3 Balance, with direct reading to 0.01 g. Top loading oranalytical style is recommended.4.4 Environments, where the mechanical pump dispenserand product will be kept during the test period.4.4.1 Ambient Area, maintained at 23 6 3C (73 6
9、5.4F).4.4.2 Oven (45C), maintained at 45 6 3C (113 6 5.4F).NOTE 2The oven temperature can be changed according to productformulation. If different temperatures are used, this should be noted in thetest report discussed in 11.1.4.4.3 Cycle Chamber, optional, alternating 5 to 50C (41 to122F) every 24
10、h.4.5 Oven-Safe Tray, with absorbent paper towels laid in thetray.4.6 Food Coloring or Dye, optional.5. Precautions5.1 Appropriate handling considerations should be given toflammable, toxic, caustic, or other potentially hazardous ma-terial used. When testing at any temperature, safety should bethe
11、number one consideration and special attention should beused on the flash points of the products tested.6. Sampling6.1 Based upon the desired precision, sampling shall beperformed in accordance with Practice E 122.1This test method is under the jurisdiction of ASTM Committee D10 onPackaging and is t
12、he direct responsibility of Subcommittee D10.33 on MechanicalDispensers.Current edition approved Oct. 1, 2005. Published November 2005. Originallyapproved in 2001. Last previous edition approved in 2001 as D 6654 01.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM
13、 Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.6.2 In the absence of any spec
14、ial sampling plan, perfor-mance shall be based on not less than the number of represen-tative specimens exposed to any of the environmental condi-tions as specified in Section 9.7. Test Specimens7.1 Test specimens shall be clean, dry, and previouslyunused mechanical pump dispensers.8. Conditioning8.
15、1 If possible, condition the test specimens at 23 6 3C (736 5.4F) for not less than 4 h. If the test specimens are notconditioned at the recommended temperature and humidity,this should be noted in the test report discussed in section 11.1.8.2 Test pumps should be tested no sooner than 24 h afterass
16、embly when possible. If pumps are not conditioned at therecommended time, this should be noted in the test reportdiscussed in 11.1.9. Test Specimen Preparation9.1 Prepare a minimum of twelve unprimed mechanicalpump dispensers with product and containers to be used forevaluation.9.1.1 Label all of th
17、e assembled units with the productname, any safety hazards for the product, name of thetechnician completing the test, and the test number or means ofidentifying the test along with the following :9.1.1.1 Minimum three units labeled, “Upright, Ambient.”9.1.1.2 Minimum three units labeled, “Upright,
18、Oven 45C”9.1.1.3 OptionalMinimum three units labeled, “Upright,Cycle Chamber.”9.1.1.4 Minimum three units labeled, “On-Side, Ambient.”9.1.1.5 Minimum three units labeled, “On-Side, Oven(45C).”9.1.1.6 OptionalMinimum three units labeled “On-Side,Cycle Chamber.”NOTE 3Since the output of this test is w
19、eight loss of product for thetotal package of container with a mechanical pump dispenser, it may beadvantages for a control package of the test container with a standardclosure to be included at each condition so that the effect of themechanical pump dispenser may be determined.10. Procedure10.1 If
20、the data is to be presented as gross weight lost only,then proceed to 10.2. If the data is to be presented as weightlost as a percentage of the weight of the product, weigh eachcontainer with its intended pump at the beginning of testingand record that data on the data sheet as “Unfilled PackagingWe
21、ight.” (Tare).10.2 Fill each container with the desired amount of product.The level of product in the container should represent the levelused for commercial use. To better identify leakage, foodcoloring or dye may be added.10.3 Affix the mechanical pump dispensers to each con-tainer securely to pre
22、vent leakage between the container at theminimum recommended torque load in accordance with TestMethod D 2063.NOTE 4It is extremely important that the test specimens exhibit theminimal recommended torque load so that the worst case for detectingleakage is observed.10.4 Weigh each package and record
23、the “initial weight”data (Wi) on a data sheet with the information identifying thepackage.10.5 Place all of the test specimens, as prepared in 9.1 intheir respective environments as indicated by the appropriatelabel on each unit. Specimens labeled “On-Side” should beplaced with the orifice facing do
24、wn excluding trigger sprayers.Trigger sprayers may have the orifice to the side. If themechanical pump dispensers use a protective hood or overcap,these test specimens should be stored without these protectivedevices in place. If the mechanical pump dispensers have alocking feature, these test speci
25、mens should be in the lockedposition during storage and the unlocked position duringinspection and testing.10.6 Once a week for a period of four weeks, (generally onthe same day of the week as the test start day), remove all ofthe test specimens from their respective environments andinspect the test
26、 specimens for leakage.10.7 Allow the temperature of the test specimens to equili-brate (generally 4-6 h) to ambient temperature prior to theactual evaluations.10.8 Weigh each package and record the “new weight” data(Wn) on the data sheet with the initial weight information.10.9 Calculate the follow
27、ing:Gross Weight Loss 5 Wi2 Wn(1)% Weight Loss 5Wi2 WnWi2 Tare3 10010.10 At the end of four weeks, evaluate the unprimedmechanical pump dispensers for each of the following param-eters:10.10.1 Final Weight LostReport the “Final Weight Lost”in accordance with 10.9.10.10.2 Strokes to PrimeReport in ac
28、cordance with TestMethod D 3890. Report the findings in 11.1.10.10.3 Output per StrokeReport in accordance with TestMethods D 4336. Report the findings in 11.1.10.11 Evaluate if the spray or the flow of the productappears to be defective or impeded. Report findings in 11.1.10.12 Retain all test spec
29、imens that are discontinued fromtesting because of one or more defects. Save these if futureexamination is required.11. Report11.1 Report the following information:11.1.1 Description of the mechanical pump dispenser (sup-plier, type, closure size, diptube length),11.1.2 Identification of the product
30、 used.11.1.3 Statement to the effect that the tests were made incompliance with this test method along with the followinginformation:11.1.3.1 Name of the technician completing the test.11.1.3.2 Date of report along with dates for the test period.11.1.4 Detailed record of test on each mechanical pump
31、dispenser as follows:D665405211.1.4.1 When a mechanical pump dispenser was discontin-ued from additional testing and the nature of its discontinu-ance;11.1.4.2 Any observations or recommendations that mayassist in correcting the various defects reported upon;11.1.4.3 Data for each package on “Initia
32、l Weight”, “NewWeight” for weeks 1, 2, 3, and 4, and “Final Weight”. Themean value and standard deviation should be calculated andreported for each variable, (for example, “Upright, Ambient”,etc.), along with the maximum and minimum values.11.1.4.4 Calculations of “Gross Weight Loss”. The meanvalue
33、and standard deviation should be calculated and reportedfor each variable, (for example, “Upright, Ambient,” etc.),along with the maximum and minimum values.11.1.4.5 If this information is desired, calculations of %weight loss. The mean value and standard deviation should becalculated and reported f
34、or each variable, (for example, “Up-right, Ambient”, etc.), along with the maximum and minimumvalues.11.1.4.6 Data for each package on strokes to prime andoutput per stroke. The mean value and standard deviationshould be calculated and reported for each variable, (forexample, “Upright, Ambient”, etc
35、.), along with the maximumand minimum values.11.2 Report the overall results of the testing and draw aconclusion as to the acceptability of the mechanical pumpdispenser. If the mechanical pump dispenser is acceptable, butwith certain limitations, note accordingly.12. Precision and Bias12.1 Precision
36、The precision of this test method is highlydependent on the particular pump style and contents tested.One laboratory has investigated one particular pump style anda hairspray product with 12 replicate tests for gross weight lossonly, yielding no visual product leakage along with the resultsprovided
37、in Table 1.12.1.1 Other pumps and contents will have other averagesand will have more or less variability between replicate tests.Users of this test method are suggested to reference historicalfiles of previous tests of similar pumps and contents for anestimate of within laboratory repeatability. Co
38、mmittee D10believes that because of this strong product and pump styledependency, further investigation of repeatability and repro-ducibility is not practicable. For the precision and bias forstrokes-to-prime and output-per-stroke data, the user shouldrefer to test methods D 3890 and D 4336.12.2 Bia
39、sThis test method has no bias because an ac-cepted reference or referee value is not available.13. Keywords13.1 mechanical pump dispenser; package; storage stabilityD6654053ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentione
40、din 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
41、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
42、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 shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C
43、700, 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).TABLE 1
44、Results from Validation TestGross Weight Loss Average Std. Dev. Max MinUpright , Ambient 0.02 0.01 0.03 0.01Upright, Oven 45C 0.25 0.02 0.29 0.23On-Side, Ambient 0.02 0.01 0.03 0.01On-side, Oven 45C 0.27 0.02 0.32 0.23% Weight Loss Average Std. Dev. Max MinUpright , Ambient NA NA NA NAUpright, Oven
45、45C NA NA NA NAOn-Side, Ambient NA NA NA NAOn-side, Oven 45C NA NA NA NAStrokes-to-Prime Average Std. Dev. Max MinUpright , Ambient 7.13 0.78 8 6Upright, Oven 45C 6.00 0.00 6 6On-Side, Ambient 7.50 0.50 8 7On-side, Oven 45C 6.13 0.33 7 6Output-per-Stroke Average Std. Dev. Max MinUpright , Ambient 0.169 0.002 0.172 0.166Upright, Oven 45C 0.167 0.002 0.170 0.165On-Side, Ambient 0.167 0.002 0.169 0.164On-side, Oven 45C 0.167 0.002 0.171 0.164D6654054
