1、Designation: D3568 03 (Reapproved 2009)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 Thermo-plastic ElastomersTensionD1646 Test Methods for RubberViscosity, Stress Relax-ation, and Pre-Vulcanization Characteristics (Mooney Vis-cometer)D2084 Test Method for Rubber PropertyVulcanizationUsing Oscillating Disk Cure MeterD2161 Practice for Conversi
6、on 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, andProcedures for Mixing Standard Compounds and Prepar-ing Standard Vulcanized She
7、etsD3896 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
8、 the Rubber and Carbon Black ManufacturingIndustriesD5289 Test Method for Rubber PropertyVulcanizationUsing Rotorless Cure MetersD6204 Test Method for RubberMeasurement of Unvul-canized Rheological Properties Using Rotorless ShearRheometers3. Significance and Use3.1 These test methods are intended m
9、ainly 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.4. Stand
10、ard 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 1.00Oil furnace blackCDSRB-B4 80.00 100.00 80.00ASTM Type 103 petroleum oilDE. 50.00
11、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 0.230.29HMIM (Banbury Head) 0.25 0.21 0.200.26H1These test methods are under the
12、 jurisdiction of ASTM Committee D11 onRubber and are the direct responsibility of Subcommittee D11.23 on SyntheticRubbers.Current edition approved Sept. 1, 2009. Published December 2009. Originallyapproved in 1977. Last previous edition approved in 2003 as D3568 03. DOI:10.1520/D3568-03R09.2For refe
13、renced 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.3The Waring blender has been found useful for this blending.4The Whip
14、mixer available from Hobart Corp., Troy, OH 45374, has been foundsatisfactory for this purpose.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.AY = partsoil by mass per 100 parts base polymer in masterbatch. If Y is greaterthan 50 pa
15、rts 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 of these materials. This“compounding material blend” is prepared by blending a proportional mass of eachmaterial, except carbon black an
16、d 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 Industry Reference Black may be used in place of NIST 378,although slightly different results may be obtained.DFor the MIM procedure, it is
17、 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 by adding a proportional mass of oil to a cavityprepared in a proportional mass of carbon black, covering the oil with thesurrounding bl
18、ack and then gently whipping until uniformly blended. Let stand 24h and blend again before using.4EViscosity is 16.8 6 1.2 mm2/s at 100C in accordance with Test Method D88and Practice D2161. Viscosity gravity constant is 0.8896 0.002 in accordance withTest Method D2501. Available in 1 and 5-gal (3.8
19、 and 19-dm3) quantities from SunOil Co. and is distributed by R. E. Carroll, P.O. Box 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
20、are available from ASTM Headquarters.GFor mill and internal mixer batches, weigh the rubber, carbon black and oil tothe nearest 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
21、 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 75 % loadingof the mixing chamber.4.1.1 Formula 1 shall apply to the general purpose EPDMtypes.4.1.2 Formula 2 shall apply to the EPDM
22、terpolymers withan ethylene content greater than approximately 67 % by mass(which describes 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 t
23、he 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 Mixing Procedure,6.1.3 Mill Procedure, and6.1.4 Internal Mixer with Final Curative Addition on MillProcedure.NOTE 1The mill handling cha
24、racteristics of the EPDM rubber aresomewhat more difficult than for most other rubbers; 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 c
25、arbon 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 Procedure:6.2.1 For general mixing procedure, refer to PracticeD3182.6.2.2 Initial Mix Cycle:Dura-tion,minAccumu-lative,minAdjust the internal
26、 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.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 t
27、he 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 isreached, whichever occurs first. Discharge thebatch.1.5 5.0Immediately pass the batch through a standardlaboratory mill, set at 50
28、6 5C (122 6 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 masterbatch for 30 min or until it is atroom temperature.Final Mix Cycle:Adjust the chamber and rotors to 40 6 5C (1046 9F). Clos
29、e 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.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, which
30、ever 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 enough sample from thebatch to allow testing of compound viscosity inaccordance with Test Methods D1646 or vulcani-zation characteri
31、stics 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 afinished thickness of approximately 2.2 mm (0.085in.). Cool on a flat, dry metal surface.For routine laboratory testing, condit
32、ion thesheeted compound for 1 to 24 h at 23 6 3C(73.46 5.4F) and a relative humidity not greaterthan 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 6 5 % relative humidity.Miniature Internal M
33、ixer (MIM) Procedure:For general mixing procedure, refer to PracticeD3182. Mix with the head temperature of the min-iature internal mixer maintained at 60 6 3C (1406 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 6 5C (122 6 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
35、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 2.0D3568 03 (2009)2Raise 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
36、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 twice at 3mm (0.125 in.) opening.6.2.2.3 Check the batch mass
37、 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. Condition the specimen for 1 to 24hat236 3C (73.4 6 5.4F) bef
38、ore 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 a specimen to allow testing of compoundedviscosity in accorda
39、nce 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 set at 50 6 5C (122 6 9F) four times, alwaysin the same direc
40、tion 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 maximum preci-sion, condition for 1 to 24 h in a closed contai
41、ner to preventabsorption of moisture from the air, or in an area controlled at35 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 po
42、ssible 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 with the mill setat 23 6 5C (73 6 9F) and 0.8 mm (0.032 in.)
43、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 is incor-porated, open the mill to 1.3 mm (0.05 in.). Makeone34 cut from each side, then add the remain-der of the mixture. When all the mixture has b
44、eenincorporated, make three34 cuts from each side.13.0 14.0NoteDo not cut any stock while free carbonblack is evident in the bank or on the milling sur-face. Be certain to return any pigments that dropthrough the mill to the milling stock.Add the accelerators and sulfur evenly acrossthe rolls still
45、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.2.0 21.06.3.2.1 Check the batch mass and record. If i
46、t 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 Method D2084 or D5289, if these are desired.6.3.2.
47、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)
48、and arelative humidity not greater than 55 %. For maximum preci-sion, condition for 1 to 24 h in a closed container to preventabsorption of moisture from the air, or in an area controlled at35 6 5 % relative humidity.6.4 Internal Mixer with Final Curative Addition on MillProcedure:6.4.1 For general
49、mixing procedure, refer to PracticeD3182.6.4.2 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 506 5C (122 6 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 t
