ASTM D6049-2003(2017) 5000 Standard Test Method for Rubber Property&x2014 Measurement of the Viscous and Elastic Behavior of Unvulcanized Raw Rubbers and Rubber Compounds by Compre.pdf

1、Designation: D6049 03 (Reapproved 2017)Standard Test Method forRubber PropertyMeasurement of the Viscous and ElasticBehavior of Unvulcanized Raw Rubbers and RubberCompounds by Compression Between Parallel Plates1This standard is issued under the fixed designation D6049; the number immediately follow

2、ing the designation indicates the year oforiginal adoption or, in the case of revision, the year of 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 i

3、s an adaptation of the GermanStandard DIN 53514, a further development of the former“Defo Test” (see Appendix X1).1.2 This test method is capable of measuring and character-izing the rheological behavior (viscosity and elasticity) ofunvulcanized raw rubbers and rubber compounds, relating tothe macro

4、 structure of rubber polymers (average molecularweight, molecular weight distribution, long chain branching,and micro- and macro-gel).1.3 The viscosity and elasticity of unvulcanized rubbers andrubber compounds are determined by subjecting cylindricaltest pieces to a compression/recovery cycle. The

5、dependencyon shear rate at constant shear stress is evaluated and thematerial fatigue behavior is determined in repeat cycle testing.1.4 The non-Newtonian viscous and elastic behavior ofrubbers and rubber compounds can also be evaluated.1.5 Statistical evaluation of the test data provides an indi-ca

6、tion of data variation, which may be employed as an estimateof the homogeneity of the material tested.1.6 The values stated in SI units are to be regarded as thestandard. The values in parentheses are for information only.1.7 This standard does not purport to address all of thesafety concerns, if an

7、y, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety, health, and environmental practices and deter-mine the applicability of regulatory limitations prior to use.1.8 This international standard was developed in accor-dance with internation

8、ally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D297 Test M

9、ethods for Rubber ProductsChemical Analy-sisD926 Test Method for Rubber PropertyPlasticity andRecovery (Parallel Plate Method)D4483 Practice for Evaluating Precision for Test MethodStandards in the Rubber and Carbon Black ManufacturingIndustriesD6048 Practice for Stress Relaxation Testing of RawRubb

10、er, Unvulcanized Rubber Compounds, and Thermo-plastic Elastomers2.2 DIN Standards:3DIN 53514 Testing of RubberDetermination of Viscosityand Elasticity Related Numbers of Raw Rubber andRubber Mixes in a Compression Test between ParallelPlatesDIN 53523, Part 1 Testing of Rubber and ElastomersTesting w

11、ith the Mooney Shearing Disk Viscometer;Preparation of Test Pieces2.3 ISO Standards:4ISO 5725 Precision of Test MethodsDetermination ofRepeatability and Reproducibility for a Standard TestMethod by Interlaboratory TestsISO 7323 RubberRaw and Unvulcanized CompoundedDetermination of Plasticity Number

12、and Recovery Num-ber; Parallel Plate Method3. Terminology3.1 DefinitionsThe following terms appear in logical or-der for the sake of clarity.3.1.1 Multiple Compression Force Testrefer to Section 10for more details.1This test method is under the jurisdiction of Committee D11 on Rubber andRubber-like

13、Materials and is the direct responsibility of Subcommittee D11.12 onProcessability Tests.Current edition approved Oct. 1, 2017. Published December 2017. Originallyapproved in 1996. Last previous edition approved in 2013 as D6049 03 (2013).DOI: 10.1520/D6049-03R17.2For referenced ASTM standards, visi

14、t 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.3Available from Deutsches Institut fr Normung, Burggrafenstr 6, D10787Berlin 30, Germany.4Availab

15、le from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized

16、principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.13.1.1.1 viscosity number, V10(Ns)the product of the forceF in N requir

17、ed to compress a test piece the final 0.5 mm (0.02in.) in a 6.0 mm (0.24 in.) total compression cycle (from 13.0to 7.0 mm (0.51 to 0.28 in.) and the compression time dt1equaling 10 s.3.1.1.2 total compression time, tTthe time in s required tocompress a test piece the full 6.0 mm (0.24 in.), that is,

18、 from13.0 to 7.0 mm (0.51 to 0.28 in.).3.1.1.3 elasticity number, DE30the elastic recovery ex-pressed in units of 0.1 mm (0.004 in.) calculated from theheight h2of the test piece after compression from 13.0 to 7.0mm (0.51 in. to 0.28 in.) within 30 s followed by a recoveryperiod of 30 s.3.1.1.4 non-

19、Newtonian viscosity exponent, n1the slope ofthe line in a double log plot of the viscosity versus the shearrate; n1is dimensionless and always negative.3.1.1.5 elasticity coeffcient, mthe slope of the line in aplot of the elasticity number DE (see 3.1.2.3) versus the log ofthe shear rate; the dimens

20、ion of m is mm (in units of 0.1 mmper decade).3.1.1.6 test data variation number, svthe average standarddeviation of the data points of the individual test pieces, fromthe regression line of the viscosity number in accordance with3.1.1.4.3.1.1.7 test data variation number, sethe average standarddevi

21、ation of the data points of the individual test pieces fromthe regression line of the elasticity number in accordance with3.1.1.5.(a) DiscussionBoth numbers, svand se, can be used to(1) characterize the homogeneity of the test pieces or (2)provide an estimate of the test precision where test pieces

22、areknown to be homogeneous. In addition, secan indicate rarecases of nonlinearity.3.1.1.8 viscous material fatigue, V21the decrease in per-cent of V10for the first compression compared to V10for thesecond compression.(a) DiscussionWhen the first compression/recoverycycle (compression time = recovery

23、 time) is repeated, theviscosity number of the second cycle will be lower than that ofthe first cycle.3.1.1.9 elastic material fatigue, Q21the quotient of therecovery times, (tRV)2and (tRV)1, after the second and firstcompression/recovery cycle, allowing the test piece to reachequivalent recovery he

24、ights in both cycles; Q21is dimension-less.(a) DiscussionIn the second compression/recoverycycle the test piece requires a longer recovery time to reach thesame height as in the first cycle.3.1.2 Single Compression Force Testrefer to Section 10for more details.3.1.2.1 viscosityspecific to this test

25、method, the ratio ofcompression force to compression time, where compressionforce and compression time are proportional to shear stress andshear rate, respectively.(a) DiscussionThe compression force F specified for aparticular material determines the deformation stress, and thecompression time dt1r

26、equired to compress a test piece the final0.5 mm (0.02 in.) in a 6.0 mm (0.24 in.) total compressioncycle (from 13.0 to 7.0 mm (0.51 to 0.28 in.) determines thedeformation rate.3.1.2.2 total compression time, tTrefer to 3.1.1.2.3.1.2.3 elastic recovery, DEcalculated from the height h2of the test pie

27、ce after compression from 13.0 to 7.0 mm (0.51in. to 0.28 in.) followed by a recovery period, equal in lengthto the compression time, expressed in units of 0.1 mm (0.004in.).3.1.2.4 non-Newtonian viscosity number, qthe quotient ofthe two compression time values dt1and tT(see 3.1.2.1 and3.1.1.2); q i

28、s dimensionless.3.1.2.5 test data variationthe standard deviations srfor thecompression time dt1(3.1.2.1) and srfor the elastic recoveryDE (3.1.2.3).(a) Discussionsee 3.1.1.7.3.1.2.6 viscous material fatigue, dt21the decrease inpercent of the compression time dt2versus the compressiontime dt1.(a) Di

29、scussionWhen the first compression/recoverycycle (compression time = recovery time) is repeated with thesame force, the compression time dt2of the second cycle willbe lower than the compression time dt1of the first cycle.4. Summary of Test Method4.1 This test method provides procedures for preparing

30、cylindrical test pieces of specified diameter and height fromunvulcanized raw rubbers and rubber compounds and fortesting their viscous and elastic behavior at a specified tem-perature in a compression/recovery operation between parallelplates.4.2 The compression device is mounted in an environmenta

31、lchamber. The preferred test temperature is 105C (221F).4.3 The change in test piece height is measured under aconstant compression force and in the recovery phase afterreleasing the force.4.4 Viscosity is characterized by compression force andcompression time, elasticity by the recovery height of t

32、he testpiece after release of the compression force (recovery phase).Material fatigue is measured through repeat compression/recovery cycles.4.5 The test can be performed with multiple compressionforces for a more comprehensive evaluation of the viscous andelastic properties, including non-Newtonian

33、 behavior, or with atime saving single compression force, preferred in qualitycontrol to test primarily uniformity of viscosity and elasticity.4.6 Statistical evaluation of the test results gives an indica-tion of data scatter, and permits also an assessment of thehomogeneity of the material under t

34、est.5. Significance and Use5.1 The viscous and elastic behavior of unvulcanized rub-bers and rubber compounds is of paramount importance inrubber manufacturing, since it affects processing, such asmixing, calendering, extrusion, and molding.The uniformity ofthese properties is equally important, as

35、fluctuations will causeupsets in manufacturing processes.D6049 03 (2017)25.2 A test capable of measuring viscosity and elasticity ofunvulcanized rubbers and rubber compounds, including theiruniformity and prediction of processing behavior, is thereforehighly desirable (see Practice D6048 for further

36、 information).5.3 Compared to many other rheological tests, this testmethod measures viscosity and elasticity related parametersunder conditions of low shear and has a high discriminatingpower. It can detect small rheological differences. A fulldiscussion of the principles behind stress relaxation t

37、esting isgiven in Practice D6048.5.4 Test results of this test method may be useful inpredicting processability, but correlation with actual manufac-turing processes must be established in each individual case,since conditions vary too widely.5.5 This test method is suitable for specification compli

38、ancetesting, quality control, referee purposes, and research anddevelopment work.6. Interferences6.1 For reliable test results it is important that test pieces areof accurate dimensions, are free of air inclusions and blisters,and contain negligible residual stresses.6.2 Although this test method is

39、 practically unlimited intesting unvulcanized rubbers, it may be necessary to considersmaller test pieces in the case of very hard and rigid sub-stances.7. Apparatus57.1 Compression Device:7.1.1 Two circular platens with a diameter of 30.0 6 0.1mm (1.181 6 0.004 in.) and a thickness of at least 2 mm

40、 (0.08in.) mounted in an angle iron frame, are facing each otherhorizontally. The upper platen can be vertically moved andraised at least 14 mm (0.55 in.) above the lower platen topermit insertion of the 13-mm (0.51-in.) high test piece.7.1.2 The upper platen shall be able to move nearly withoutfric

41、tion, that is, it must smoothly descend under the contactforce specified in 7.1.5.7.1.3 The upper platen shall be capable of applying acompressive force between 1 and 800 N (0.22 and 180 lbf) 60.5 % to the test piece within 1 s. The force should be appliedrapidly but not abruptly.7.1.4 After the hei

42、ght of the test piece has been reducedfrom 13.0 to 7.0 mm (0.51 to 0.28 in.) the compression forceshall be released in less than 0.5 s.7.1.5 A residual compression force of 0.040 6 0.005 N(0.009 6 0.001 lbf) shall always be maintained by the upperplaten to warrant an intimate contact with the test p

43、iece prior tocompression and during the recovery cycle. The mass of theupper platen must be taken into account and compensated for.7.1.6 The position of the upper platen shall be continuouslyrecorded during the test to the nearest 0.01 mm (0.0004 in.) inat least 0.05 s intervals. The starting time o

44、f the compressioncycle, the time of reaching compression heights of 7.5 and 7.0mm (0.30 and 0.28 in.), and the recovery times shall berecorded to the nearest 0.05 s.7.1.7 The compressed test pieces shall only be in contactwith the two platens and the platens shall be kept free ofcontamination. The t

45、est piece arrangement is illustrated in Fig.1.7.2 Test Chamber:7.2.1 The compression device shall be contained in a testchamber that can be temperature controlled between 20 and170 6 1C (68 and 338 6 2F).7.2.2 The test chamber shall have holding devices to ac-commodate test pieces of 13.0 6 0.1 mm (

46、0.51 6 0.004 in.)plus twice the thickness of the sandpaper in height forconditioning.7.3 Recording and Evaluation of Test Results:7.3.1 The test shall be run and controlled automatically,including recording of the compression heights and times.7.3.2 Evaluation of test results is best carried out imm

47、edi-ately after the test. The use of a computer to control the testsequence and record data is recommended.8. Preparation of Test Pieces8.1 The cylindrical test piece shall have a height of 13.0 60.1 mm (0.51 6 0.004 in.) and a diameter of 30.0 6 0.1 mm(1.18 6 0.004 in.). It is typically produced by

48、 molding andshould be free of blisters and internal residual stresses. Sand-paper disks6shall be molded to the top and bottom of thecylindrical test piece to stabilize the surfaces and ensure aneven transmission of the compression forces without slippage.The sandpaper facing also prevents fouling of

49、 the platens of thecompression device and can be used for identification pur-poses.8.2 Test Pieces from Rubber in Bale Form:8.2.1 Sheets of approximately 2 mm (0.08 in.) in thicknessare sliced from the bale, and disks of approximately 30 mm(1.18 in.) in diameter are die cut from these sheets. The disks5A suitable instrument can be obtained under the name Defo-Elastometer(System Bayer) from Haake, Inc., West Century Road, Paramus, NJ 07652, orHaake G.m.b.H., Dieselstr., D76227 Karlsruhe, Germany.6A suitable sandpaper is 3M 230N (120 grit, al