ASTM D3568-2003(2018) Standard Test Methods for Rubber&x2014 Evaluation of EPDM (Ethylene Propylene Diene Terpolymers) Including Mixtures With Oil.pdf

1、Designation: D3568 03 (Reapproved 2018)Standard Test Methods forRubberEvaluation of EPDM (Ethylene Propylene DieneTerpolymers) Including Mixtures With Oil1This standard is issued under the fixed designation D3568; the number immediately following the designation indicates the year oforiginal adoptio

2、n 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 These test methods specify the standard materials, testformulas, mixing pro

3、cedures, and test methods for the evalu-ation and production control of ethylene propylene dienerubbers (EPDM).1.2 The values stated in SI units are to be regarded as thestandard. The values in parentheses are for information only.1.3 This standard does not purport to address all of thesafety concer

4、ns, if any, 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.1.4 This international standard was developed in accor-dance with in

5、ternationally 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:2D8

6、8 Test Method for Saybolt ViscosityD412 Test Methods for Vulcanized Rubber and Thermoplas-tic ElastomersTensionD1646 Test Methods for RubberViscosity, StressRelaxation, and Pre-Vulcanization Characteristics(Mooney Viscometer)D2084 Test Method for Rubber PropertyVulcanizationUsing Oscillating Disk Cu

7、re MeterD2161 Practice for Conversion of Kinematic Viscosity toSaybolt Universal Viscosity or to Saybolt Furol ViscosityD2501 Test Method for Calculation of Viscosity-GravityConstant (VGC) of Petroleum OilsD3182 Practice for RubberMaterials, Equipment, and Pro-cedures for Mixing Standard Compounds a

8、nd PreparingStandard Vulcanized SheetsD3896 Practice for Rubber From Synthetic SourcesSamplingD3900 Test Methods for RubberDetermination of Ethyl-ene Units in Ethylene-Propylene Copolymers (EPM) andin Ethylene-Propylene-Diene Terpolymers (EPDM) byInfrared SpectrometryD4483 Practice for Evaluating Pr

9、ecision for Test MethodStandards in the Rubber and Carbon Black ManufacturingIndustriesD5289 Test Method for Rubber PropertyVulcanizationUsing Rotorless Cure MetersD6204 Test Method for RubberMeasurement of Unvulca-nized Rheological Properties Using Rotorless Shear Rhe-ometers3. Significance and Use

10、3.1 These test methods are intended mainly for refereepurposes but may be used for quality control of rubberproduction. They may also be used in research and develop-ment work and for comparison of different rubber samples in astandard formula.3.2 These test methods may be used to obtain values forc

11、ustomer acceptance of rubber.1These test methods are under the jurisdiction of ASTM Committee D11 onRubber and Rubber-like Materials and are the direct responsibility of SubcommitteeD11.23 on Synthetic Rubbers.Current edition approved June 1, 2018. Published August 2018. Originallyapproved in 1977.

12、Last previous edition approved in 2013 as D3568 03 (2013).DOI: 10.1520/D3568-03R18.2For referenced 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 pa

13、ge onthe ASTM website.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 principles on standardization established in the Decision on Principles for t

14、heDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.14. Standard Test Formulas4.1 Standard Formulas:3,4MaterialFormula No.NISTSRM/IRMNo.QualityParts by Mass12 3EPDM . 100.00 100.00 100.00 + YAZinc oxi

15、deBIRM 91 5.00 5.00 5.00SulfurB371 1.50 1.50 1.50Stearic acidB372 1.00 1.00 1.00Oil furnace blackCDSRB-B4 80.00 100.00 80.00ASTM Type 103 petroleum oilDE. 50.00 75.00 50.00 YATetramethylthiuramdisulfide (TMTD)BIRM 1F1.00 1.00 1.00Mercaptobenzothiazole(MBT)B383 0.50 0.50 0.50Total 239.00 284.00 239.0

16、0Batch factorGMill 2.0 2.0 2.0Internal mixer 5.5 4.2 5.5MIM (Cam Head) 0.29 0.25 0.230.29HMIM (Banbury Head) 0.25 0.21 0.200.26HAY = partsoil by mass per 100 parts base polymer in masterbatch. If Y is greaterthan 50 parts oil, do not add oil to Formula 3.BFor the MIM procedure, it is recommended tha

17、t a blend of compoundingmaterials be prepared to improve accuracy in the weighing of these materials. This“compounding material blend” is prepared by blending a proportional mass of eachmaterial, except carbon black and oil, in a dry powder blender such as a biconicalblender or vee blender. A mortar

18、 and pestile or blender may be used for blendingsmall quantities.3CThe current Industry Reference Black may be used in place of NIST 378,although slightly different results may be obtained.DFor the MIM procedure, it is recommended that a blend of carbon black and oilbe prepared to improve accuracy i

19、n the weighing and addition of these materials.This “black/oil blend” is prepared by adding a proportional mass of oil to a cavityprepared in a proportional mass of carbon black, covering the oil with thesurrounding black and then gently whipping until uniformly blended. Let stand 24h and blend agai

20、n before using.4EViscosity is 16.8 1.2 mm2/s at 100C in accordance with Test Method D88 andPractice D2161. Viscosity gravity constant is 0.889 0.002 in accordance with TestMethod D2501. Available in 1 and 5-gal (3.8 and 19-dm3) quantities from Sun OilCo. and is distributed by R. E. Carroll, P.O. Box

21、 139, Trenton, NJ 08601.FNIST has discontinued supply of SRM 374. A substitute material is available asIRM 1 from Forcoven Products, Inc., P.O. Box 1556, Humble, TX 77338. Ref-erence to research reports RR D04-1034 are available from ASTM Headquarters.GFor mill and internal mixer batches, weigh the

22、rubber, carbon black and oil to thenearest 1.0 g, the sulfur and accelerators to the nearest 0.02 g, and all othercompounding materials to the nearest 0.1 g. For MIM batches, weigh the rubberand compounding material blend to the nearest 0.01 g and individual compoundingmaterial, if used, to the near

23、est 0.001 g.HCalculate a batch factor to the nearest 0.01, which will provide a 75 % loading ofthe mixing chamber.4.1.1 Formula 1 shall apply to the general purpose EPDMtypes.4.1.2 Formula 2 shall apply to the EPDM terpolymers withan ethylene content greater than approximately 67 % by mass(which des

24、cribes high green-strength extrusion grade rubbers).For determining ethylene content, refer to Test MethodsD3900.4.1.3 Formula 3 shall apply to oil extended EPDM rubbers.5. Sample Preparation5.1 Obtain and prepare the test samples in accordance withPractice D3896.6. Mixing Procedures6.1 Four mixing

25、procedures are offered:6.1.1 Internal Mixer Procedure,6.1.2 Miniature Internal Mixing Procedure,6.1.3 Mill Procedure, and6.1.4 Internal Mixer with Final Curative Addition on MillProcedure.NOTE 1The mill handling characteristics of the EPDM rubber aresomewhat more difficult than for most other rubber

26、s; therefore, mixing isaccomplished more easily in an internal mixer. Results from mill mixingin some instances may not correlate with results obtained from internalmixer procedures. Unless it is certain that good carbon black dispersionwill be obtained by the mill mixing procedure with the rubber u

27、nder test,the internal mixer procedures shall be used.6.2 Internal Mixer Procedure:6.2.1 For general mixing procedure, refer to PracticeD3182.6.2.2 Initial Mix Cycle:Dura-tion,minAccumu-lative,minAdjust the internal mixer temperature to achievethe discharge conditions outlined in 6.2.2.4. Closethe d

28、ischarge gate, start the rotors at 8.0 rad/s(77 r/min), and raise the ram.00Charge the rubber, zinc oxide, carbon black, oil,and stearic acid. Lower the ram, start the timer,and allow the batch to mix.3.0 3.0Raise the ram and clean the mixer throat andthe top of the ram. Lower the ram.0.5 3.5Allow t

29、he batch to mix until a temperature of150C (302F) or a total mixing time of 5 min isreached, whichever occurs first. Discharge thebatch.1.5 5.0Immediately pass the batch through a standardlaboratory mill, set at 50 5C (122 9F) withan opening of 2.5 mm (0.10 in.).Check the batch mass and record. If i

30、t differsfrom the theoretical value by more than 0.5 %,discard the batch.Cool the masterbatch for 30 min or until it is atroom temperature.Final Mix Cycle:Adjust the chamber and rotors to 40 5C (104 9F). Close the discharge gate, start the rotorsat 8 rad/s (77 r/min), and raise the ram.00Charge one

31、half of the batch, accelerators andsulfur, and the remaining portion of the batch.Lower the ram.0.5 0.5Allow the batch to mix until a temperature of110C (230F) or a total mixing time of 2 min isreached, whichever occurs first. Discharge thebatch.1.5 max 2.0 maxCheck the batch mass and record. If it

32、differsfrom the theoretical value by more than 0.5 %,discard the batch. Cut enough sample from thebatch to allow testing of compound viscosity inaccordance with Test Methods D1646 or vulcani-zation characteristics in accordance with TestMethod D2084, or both, if these are desired.If stress-strain te

33、sting is to be conducted, sheetoff the stock from the mill at a setting to give afinished thickness of approximately 2.2 mm (0.085in.). Cool on a flat, dry metal surface.For routine laboratory testing, condition thesheeted compound for 1 to 24 h at 23 3C(73.4 5.4F) and a relative humidity not greate

34、rthan 55 %. For maximum precision, condition for1 to 24 h in a closed container to prevent absorp-tion of moisture from the air, or in an area con-trolled at 35 5 % relative humidity.Miniature Internal Mixer (MIM) Procedure:3The Waring blender has been found useful for this blending.4The Whip mixer

35、available from Hobart Corp., Troy, OH 45374, has been foundsatisfactory for this purpose.D3568 03 (2018)2For general mixing procedure, refer to PracticeD3182. Mix with the head temperature of the min-iature internal mixer maintained at 60 3C (140 5F) and rotor speed at6.3 to 6.6 rad/s (60 to 63 r/mi

36、n).Mixing Cycle:Prepare the rubber by pass-ing it through a mill one time with the temperatureset at 50 5C (122 9F) and an opening thatwould give an approximately 5 mm (0.2 in.) thicksheet. Cut into strips that are approximately 25mm (1 in.) wide.Charge the mixing cham-ber with the rubber strips, lo

37、wer the ram, and startthe timer.00Masticate the rubber. 1.0 1.0Raise the ram and add the zinc oxide, sulfur,stearic acid, TMTD, and MBT that have previouslybeen blended, taking care to avoid any loss.Sweep the orifice and lower the ram.1.0 2.0Raise the ram and add the carbon black/oilblend, lower th

38、e ram and allow the batch to mix.7.0 9.06.2.2.1 Turn off the motor, raise the ram, remove the mixingchamber, and discharge the batch. Record the maximum batchtemperature indicated, if desired.6.2.2.2 Pass the batch through the mill set at 50 6 5C (1226 9F) and 0.5 mm (0.020 in.), opening once, then

39、twice at 3mm (0.125 in.) opening.6.2.2.3 Check the batch mass and record. If it differs fromthe theoretical value by more than 0.5 %, discard the batch.6.2.2.4 Cut a specimen for testing of vulcanization charac-teristics in accordance with Test Method D2084 or D5289 asdescribed in 7.1, if required.

40、Condition the specimen for 1 to 24hat236 3C (73.4 6 5.4F) before testing.6.2.2.5 If either compounded viscosity or stress-strain test,or both are required, pass the rolled stock endwise through themill six times with the mill rolls set at 50 6 5C (122 6 9F)and 0.8 mm (0.032 in.) opening.6.2.2.6 Cut

41、a specimen to allow testing of compoundedviscosity in accordance with Test Methods D1646 if required.6.2.2.7 If tensile stress is required, sheet off the compoundfrom the mill at a setting to give a finished gage of approxi-mately 2.2 mm (0.085 in.) by passing the folded stock betweenthe mill rolls

42、set at 50 6 5C (122 6 9F) four times, alwaysin the same direction to obtain the effects of mill direction.Cool on a flat, dry metal surface.6.2.2.8 For routine laboratory testing, condition the sheetedcompound for 1 to 24 h at 23 6 3C (73.4 6 5.4F) and arelative humidity not greater than 55 %. For m

43、aximumprecision, condition for 1 to 24 h in a closed container toprevent absorption of moisture from the air, or in an areacontrolled at 35 6 5 % relative humidity.6.3 Mill Mix Procedure (Note 1):6.3.1 For general mixing procedure, refer to PracticeD3182.6.3.2 Mixing Cycle:NOTE 2The indicated mill o

44、penings are desired and should bemaintained in so far as possible to provide a good rolling bank at the nipof the rolls during mixing.NOTE 3Mix the zinc oxide, carbon black, stearic acid, and oil togetherbefore starting to mill the mix.Dura-tion,minAccumu-lative,minBand the rubber on the fast roll w

45、ith the mill setat 23 5C (73 9F) and 0.8 mm (0.032 in.)opening.1.0 1.0Add the mixture of zinc oxide, carbon black,stearic acid, and oil evenly across the mill with aspatula. When about half of the mixture isincorporated, open the mill to 1.3 mm (0.05 in.).Make one34 cut from each side, then add ther

46、emainder of the mixture. When all the mixturehas been incorporated, make three34 cuts fromeach side.13.0 14.0NOTE 1Do not cut any stock while freecarbon black is evident in the bank or on themilling surface. Be certain to return any pig-ments that drop through the mill to the millingstock.Add the ac

47、celerators and sulfur evenly acrossthe rolls still set at 1.3 mm (0.05 in.) opening.3.0 17.0Make three34 cuts from each side, allowing 15 sbetween each cut.2.0 19.0Cut the stock from the mill. Set the mill openingat 0.8 mm (0.032 in.) and pass the rolled stockthrough the opening endwise six times.2.

48、0 21.06.3.2.1 Check the batch mass and record. If it differs fromthe theoretical value by more than 0.5 %, discard the batch.6.3.2.2 Cut a specimen to allow testing of compoundviscosity in accordance with Test Methods D1646 or TestMethod D6204, or vulcanization characteristics in accordancewith Test

49、 Method D2084 or D5289, if these are desired.6.3.2.3 If stress-strain testing is to be conducted, sheet offthe stock from the mill at a setting to give a finished thicknessof approximately 2.2 mm (0.085 in.). Cool on a flat, dry metalsurface.6.3.2.4 For routine laboratory testing, condition the sheetedcompound for 1 to 24 h at 23 6 3C (73.4 6 5.4F) and arelative humidity not greater than 55 %. For maximumprecision, condition for 1 to 24 h in a closed container toprevent absorption of moisture from the air, o