1、Designation: F 119 82 (Reapproved 2008)Standard Test Method forRate of Grease Penetration of Flexible Barrier Materials(Rapid Method)1This standard is issued under the fixed designation F 119; the number immediately following the designation indicates the year oforiginal adoption or, in the case of
2、revision, the year of last revision. 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 test meth
3、od provides standard conditions for deter-mining the rate of grease penetration of flexible barriermaterials. Pinholes, which can be measured by a separate test,will increase the rate of grease penetration as determined bythis test method.1.2 The values stated in SI units are to be regarded as thest
4、andard. The values given in parentheses are for informationonly.1.3 This standard does not purport to address the safetyconcerns associated with its use. It is the responsibility of theuser of this standard to establish appropriate safety and healthpractices and determine the applicability of regula
5、tory limita-tions prior to use.2. Referenced Documents2.1 ASTM Standards:2D 374 Test Methods for Thickness of Solid Electrical Insu-lationD 618 Practice for Conditioning Plastics for TestingD 1898 Practice for Sampling of Plastics32.2 TAPPI Standard:TAPPI T465 sm-52 Creasing of Paper for Water Vapor
6、Permeability Tests43. Summary of Test Method3.1 Flexible barrier materials, uncreased or creased by astandard procedure, are exposed on one side to grease con-tained in a weighted cotton patch. The time required to show avisual change caused by wetting (reduction in light scattering)of a ground-glas
7、s back-up plate is measured.4. Significance and Use4.1 This test method is valuable in the development andselection of flexible barrier materials suited for use as greasebarriers.4.2 The test is rapid in comparison with other methodsbecause of the extremely small quantity of oil required fordetectio
8、n (about 6 g). The actual time to failure is a multipleof the values obtained by this test method. When permeation isthrough an absorbent structure such as kraft paper coated withpolyethylene, the failure times will be longer and variable,depending on the variation in porosity and thickness of thest
9、ructure.5. Apparatus5.1 Backing Plates, ground-glass, 50 by 50 by 3-mm (2 by2by18-in.), very fine grind on one side only.NOTE 1The ground-glass backing plates may be prepared from 2 by2-in. squares of18-in. plate glass by lightly grinding the surface with asilicon carbide abrasive as follows: Place
10、a piece of plate glass approxi-mately 1ft square on a flat surface. Mix some abrasive and water in smallquantities to make a fairly uniform paste. Place one of the 2-in. squares ofplate glass face down in the abrasive paste, and rotate it in a figure eightmovement with the finger tips using the slig
11、htest amount of pressure.When the paste gets too heavy, remove the plate glass square from the bedand wash it to remove all traces of abrasive. Add more water to the thickabrasive paste on the bed. (If necessary, add small amounts of abrasive.)Continue the process until a uniform and light overall e
12、tch is present onthe face of the square. When a uniform etch has been obtained, wash thesquare thoroughly to remove all traces of abrasive and pat dry with lenstissue.5.2 Weights, 50-g, 20 mm (0.75 in.) in diameter at the base.5.3 Patches, rifle cleaning, cotton flannel.5.4 Medicine dropper.5.5 Forc
13、ed-Circulation Oven, designed to maintain a testtemperature of 40 or 60C within 61C.5.6 Creasing Surface, consisting of a flat rectangular plate(for example, a piece of machined metal plate about 10 mmthick or a piece of plate glass) with a width at least 75 mm (3in.) on all sides.1This test method
14、is under the jurisdiction ofASTM Committee F02 on FlexibleBarrier Packaging and is the direct responsibility of Subcommittee F02.10 onPermeation.Current edition approved April 1, 2008. Published April 2008. Originallyapproved in 1970. Last previous edition approved in 2002 as F 119 82 (2002).2For re
15、ferenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Withdrawn.4Available from Technical Association of the Pulp and Pap
16、er Industry (TAPPI),15 Technology Parkway South, Norcross, GA 30092, http:/www.tappi.org.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5.7 Creasing Platen, consisting of a 5.5-kg (12-lb) squaremetal bar with 65-mm (2.5-in.) sides a
17、nd a flat base.NOTE 2The developers of this method believe that a standard creaseis easier to obtain with a flat platen than with a roller. The weight of theplaten was selected to conform to the weight loading per inch of crease inTAPPI T465 sm-52.5.8 Flat Strip of wood or metal to give the specimen
18、 apreliminary light crease.5.9 Thickness Measuring Device, capable of measuringthickness of specimens in compliance with Test MethodsD 374.6. Reagents6.1 Animal Oil (lard).6.2 Mineral Oil.6.3 Vegetable Oil.6.4 Other reagents, such as butter, tallow, and oils. Thesemay be substituted for standard rea
19、gents listed above tosimulate actual end-use conditions. Standard reagents are,however, recommended for purposes of interlaboratory com-parisons.7. Sampling, Test Specimens, and Test Unit7.1 No single procedure for sampling is adequate for allsituations. Sampling, however, should be designed to prov
20、idethe desired result in each situation. Therefore, Practice D 1898is recommended as a guide in designing appropriate samplingprocedures for the purposes at hand.7.2 Flat SpecimenCut a minimum of three test specimens60 by 60 mm (238 by 238 in.) from each sample afterconditioning at least 40 h at 23
21、6 2C and 50 6 5 % relativehumidity. Measure the thickness of each specimen in fiveequally spaced positions as described in Test Methods D 374 tothree significant figures, or to 0.00025 mm (0.01 mil) whenthree significant digits cannot be obtained. Record the mea-surements.7.3 Crease TestPrepare a mi
22、nimum of six test specimensas described in 7.2. Fold three specimens with top side up andthree specimens with bottom side up. Fold through the centerparallel to one side and press a flat strip of wood or metal downon the fold to give the specimen a preliminary light crease. Tiltthe 5.5-kg (12-lb) cr
23、easing platen and slip the folded specimenunder it and parallel to its edge, until the fold lies at the centerof gravity of the platen. Gently lower the platen and let it reston the specimen for 15 s. Remove the specimen and unfold it.Then fold it on the same side to make a new crease at a 90angle t
24、o the first crease, following the same procedure. Flattenthe specimen by unfolding it and placing it under platen for 15s.7.4 Test UnitAminimum of three similar specimens makeup a test unit.8. Procedure8.1 Place the test specimen of measured thickness on a cleanground-glass backing plate. The film s
25、pecimen should morethan cover the glass backing plate so premature edge creepfailure does not occur. Test specimens should include flat,creased into, and creased away from the side that will comeinto contact with grease in the package.NOTE 3Previously used ground-glass backing plates should be thor-
26、oughly cleaned by allowing them to stand overnight in a chromic acidsolution.8.2 Cut the cotton flannel rifle cleaning patches into 20-mm(0.75-in.) diameter disks to just fit under the 50-g weight.8.3 Place two cotton flannel disks on top of each other at thecenter of the test specimen.8.4 Place the
27、 50-g weight on the patches and preheat theentire assembly (glass, test specimen, cotton disks, and weight)to the desired test temperature (40 or 60 61C) for 30 min.This is particularly necessary when short failure times areexpected, where 630 min would be critical.8.5 With the assembly still in the
28、 oven, remove the weightsand add six drops of reagent, oil, or grease, to the cotton disks.If necessary, melt the grease so it can be added dropwise.Periodic addition may be required when volatile reagents areused under the option of 6.4.8.6 Replace the 50-g weights on the oiled patches.8.7 Close th
29、e oven door and note the time.8.8 At periodic intervals, depending on the length of time toanticipated failure (that is, every 15 min for the first hour;every 30 min for the next 4 h; then at convenient intervals), liftthe test specimen, cotton disk, and weight from the ground-glass plate as a unit
30、and observe the surface of the glass againsta dark background. Record the time at which the first trace ofwetting (reduction in light scattering) is visible at the positionof the weight. If no failure is visible, replace the assembly inthe oven.8.9 If failure as indicated by the first visible wettin
31、g occursin less than 1 h at elevated temperatures, the disruption intemperature by the act of observing the sample is sufficient toalter the end point significantly. In these cases repeat the testand check the end point at different times for each of severaltests until failure time is obtained.9. Ca
32、lculation9.1 Calculate the average and standard deviation of thethickness measurements from each specimen and record them.10. Report10.1 The report shall include the following information:10.1.1 Complete sample identification.10.1.2 Type specimen used, that is, flat or creased, and thesize of the te
33、st unit.10.1.3 Type of reagent used.10.1.4 Test temperature.10.1.5 Thickness, average, and standard deviation for eachspecimen tested.10.1.6 Average time to failure plus the minimum andmaximum time to failure for each sample with the samplesnominal thickness.11. Precision11.1 The data presented here
34、 were calculated from theresults of a round robin participated in by five laboratories.55Supporting data describing the work of the Round-Robin Task Group areavailable from ASTM International Headquarters. Request RR-F02-0001.F 119 82 (2008)2The test covered four substrates: 1 and 2 mil low-densityp
35、olyethylene (LDPE) film; 0.75 mil polypropylene homopoly-mer film; 1 mil low-density polyethylene on 40-lb kraft paper.Oils tested were mineral oil and vegetable oil. Substrates weretested flat, creased into oil and creased away from oil. The testtemperature was 60C.11.2 The results of the round rob
36、in showed an overall onesigma standard deviation of 31 % for uncreased samples. Nosignificant differences in the average results were observed oncreasing the samples before testing. This is an excellentagreement considering: (1) the large dependency of oil perme-ation on temperature (61C test temper
37、ature = 14 to + 18 %deviation); (2) film thickness (1.25 6 0.1 mil = 613 % devia-tion); (3) that this was the first time most of the laboratories hadrun the test; and (4) the test end point is not read continuously,but at intervals. Even so, this permeation test can distinguishbetween 1 and 2 mils o
38、f polyethylene rather than merely rankmaterials by decade differences.NOTE 4The dependence of mineral oil permeation on temperatureand film thickness was determined separately by one of the round-robintesting laboratories. The effect of film thickness is obtained from empiricalmeasurements which res
39、ulted in the following equation:P2P15St2t1D1.635(1)where:P = time to failure, andt = film thickness.This relationship was obtained on films of two differentmaterials (low-density polyethylene and ionomer) at 23, 40,and 60C over a range of thicknesses of 0.5 to 4.0 mils.11.3 Repeatability (Within-Lab
40、oratory)Each laboratorymade three determinations simultaneously on each substrateand oil combination. At least 82 % of the time each sample inthese triplicate determinations gave identical values.11.4 Reproducibility (Between-Laboratories)The datashowed an overall standard deviation of 31 % (uncreas
41、edsamples) from the average values reported by each laboratory.The standard deviations ranged from 19.4 to 46.4 % betweenlaboratories for each substrate and oil tested. No significantchange in the average values could be attributed to creasing theparticular samples used in this round robin.11.5 The
42、round-robin data resulted in the following average( X) and range of permeation times among the testing labora-tories:Hours to Failure, 60CSubstrateMineralOilVegetableOilLDPE, 1 mil X0.375 1.58LDPE, 2 milrangeX0.25 to 0.50.9050.9to2.02.30range 0.4 to 1.5 1.5 to 3.0Polypropylene, X17.5 2640.75 mil ran
43、ge 14 to 22 168 to 356LDPE/40-lbKraft, 1 milXrange15.212 to 2038.327 to 5012. Keywords12.1 flexible barrier packaging; grease penetrationASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this sta
44、ndard 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 must be reviewed every five years an
45、dif 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,
46、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, 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).F 119 82 (2008)3
