1、Designation: D3568 03 (Reapproved 2013)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 and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D88 Test Method for Saybolt ViscosityD412
5、 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 Cure MeterD2161 Practice for Conversion o
6、f 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 and PreparingStandard Vulcanized SheetsD
7、3896 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 Precision for Test MethodStandards in the
8、 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 Use3.1 These test methods are intended mai
9、nly 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 forcustomer acceptance of rubber.1These tes
10、t methods are under the jurisdiction of ASTM Committee D11 onRubber and are the direct responsibility of Subcommittee D11.23 on SyntheticRubbers.Current edition approved Nov. 1, 2013. Published January 2014. Originallyapproved in 1977. Last previous edition approved in 2009 as D3568 03 (2009).DOI: 1
11、0.1520/D3568-03R13.2For 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 page onthe ASTM website.Copyright ASTM International, 100 Barr Har
12、bor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States14. Standard Test Formulas4.1 Standard Formulas:3,4MaterialFormula No.NISTSRM/IRMNo.QualityParts by Mass12 3EPDM . 100.00 100.00 100.00 + YAZinc oxideBIRM 91 5.00 5.00 5.00SulfurB371 1.50 1.50 1.50Stearic acidB372 1.00 1.00 1.00O
13、il 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 239.00 284.00 239.00Batch factorGMill 2.0 2.0 2.0Internal mixer 5.5 4.2 5.5MIM (Cam Head) 0.29 0.25
14、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 that a blend of compoundingmaterials be prepared to improve accuracy in the weighing
15、 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 and pestile or blender may be used for blendingsmall quantities.3CThe current In
16、dustry 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 in the weighing and addition of these materials.This “black/oil blend” is prepared
17、 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 again before using.4EViscosity is 16.8 1.2 mm2/s at 100C in accordance with Test Meth
18、od 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 139, Trenton, NJ 08601.FNIST has discontinued supply of SRM 374. A substitute ma
19、terial 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 rubber, carbon black and oil to thenearest 1.0 g, the sulfur and accelerators to
20、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 nearest 0.001 g.HCalculate a batch factor to the nearest 0.01, which will provide a 7
21、5 % 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 describes high green-strength extrusion grade rubbers).For determining ethylene cont
22、ent, 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 procedures are offered:6.1.1 Internal Mixer Procedure,6.1.2 Miniature Internal Mi
23、xing 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 rubbers; therefore, mixing isaccomplished more easily in an internal mixer. Results fro
24、m 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 under test,the internal mixer procedures shall be used.6.2 Internal Mixer Procedur
25、e: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 discharge gate, start the rotors at 8.0 rad/s(77 r/min), and raise the ram.00Charg
26、e 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 the batch to mix until a temperature of150C (302F) or a total mixing time of 5 min
27、 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 it differsfrom the theoretical value by more than 0.5 %,discard the batch.Cool the
28、 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 half of the batch, accelerators andsulfur, and the remaining portion of the batch
29、.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 differsfrom the theoretical value by more than 0.5 %,discard the batch. Cut enoug
30、h 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 testing is to be conducted, sheetoff the stock from the mill at a setting to give a
31、finished 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 greaterthan 55 %. For maximum precision, condition for1 to 24 h in a closed container t
32、o 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 available from Hobart Corp., Troy, OH 45374, has been foundsatisfactory for this
33、purpose.D3568 03 (2013)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/min).Mixing Cycle:Prepare the rubber by pass-ing it through a mill one time with th
34、e 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, lower the ram, and startthe timer.00Masticate the rubber. 1.0 1.0Raise the ram and
35、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 the ram and allow the batch to mix.7.0 9.06.2.2.1 Turn off the motor, raise the ram
36、, 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 twice at 3mm (0.125 in.) opening.6.2.2.3 Check the batch mass and record. If it d
37、iffers 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. Condition the specimen for 1 to 24hat236 3C (73.4 6 5.4F) before testing.6.2.2.5
38、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 a specimen to allow testing of compoundedviscosity in accordance with Test Method
39、s 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 set at 50 6 5C (122 6 9F) four times, alwaysin the same direction to obtain the e
40、ffects 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 maximumprecision, condition for 1 to 24 h in a closed container toprevent absorpti
41、on 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 openings are desired and should bemaintained in so far as possible to provide a go
42、od 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 with the mill setat 23 5C (73 9F) and 0.8 mm (0.032 in.)opening.1.0 1.0Add the mix
43、ture 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 theremainder of the mixture. When all the mixturehas been incorporated, make three34
44、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 accelerators and sulfur evenly acrossthe rolls still set at 1.3 mm (0.05 in.) openi
45、ng.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.2.0 21.06.3.2.1 Check the batch mass and record. If it differs fromthe theoretical
46、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 Method D2084 or D5289, if these are desired.6.3.2.3 If stress-strain testing is
47、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 gre
48、ater than 55 %. For maximumprecision, 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.6.4 Internal Mixer with Final Curative Addition on MillProcedure:6.4.1 For general mixing procedure, refer to Pract
49、iceD3182.6.4.2 Initial Mix Cycle in Internal Mixer:6.4.2.1 Follow the mix cycle stated in 6.2.2.1 to 6.2.2.7.6.4.3 Final Mix Cycle on Mill:6.4.3.1 The mill batch mass shall be based on twice theformula mass.Dura-tion,minAccumu-lative,minSet the mill temperature at 50 5C (122 9F)with a mill opening of 1.5 mm (0.06 in.). Band themasterbatch on the fast roll and add the sulfurand accelerators evenly across the rolls.1.0 1.0Make three |n cuts from each side, allowing 15s between each cut.2.0 3.0Cut the bat
