1、Designation: D 3568 03Standard Test Methods forRubberEvaluation of EPDM (Ethylene Propylene DieneTerpolymers) Including Mixtures With Oil1This standard is issued under the fixed designation D 3568; the number immediately following the designation indicates the year oforiginal adoption or, in the cas
2、e of 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.1. Scope1.1 These test methods specify the standard materials, testformulas, mixing procedures, and te
3、st 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 concerns, if any, ass
4、ociated 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:2D 88 Test Method for Saybolt ViscosityD 412 Test Methods
5、 for Vulcanized Rubber and Thermo-plastic Elastomers TensionD 1646 Test Methods for RubberViscosity, Stress Relax-ation, and Pre-Vucanization Characteristics (Mooney Vis-cometer)D 2084 Test Method for Rubber PropertyVulcanizationUsing Oscillating Disk Cure MeterD 2161 Practice for Conversion of Kine
6、matic Viscosity toSaybolt Universal Viscosity or to Saybolt Furol ViscosityD 2501 Test Method for Calculation of Viscosity-GravityConstant (VGC) of Petroleum OilsD 3182 Practice for RubberMaterials, Equipment, andProcedures for Mixing Standard Compounds and Prepar-ing Standard Vulcanized SheetsD 389
7、6 Practice for Rubber from Synthetic SourcesSamplingD 3900 Test Methods for Rubber RawDetermination ofEthylene Units in EPM (Ethylene-Propylene Copolymers)and EPDM (Ethylene-Propylene-Diene Terpolymers)D 4483 Practice for Determining Precision for Test MethodStandards in the Rubber and Carbon Black
8、IndustriesD 5289 Test Method for Rubber PropertyVulcanizationUsing Rotorless Cure MetersD 6204 Test Method for RubberMeasurement of Unvulca-nized Rheological Properties Using Rotorless Shear Rhe-ometers3. Significance and Use3.1 These test methods are intended mainly for refereepurposes but may be u
9、sed 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. Standard Test Formulas4.1 Standard Formulas
10、: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 75.00 50.00 YATetramethylthiuramdisulf
11、ide (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 0.200.26HAY = partsoil by mass per 100 parts base polymer in masterbatch. If Y i
12、s 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 of these materials. This1These test methods are under the jurisdiction of ASTM Committee D11 onRubber and are the dir
13、ect responsibility of Subcommittee D11.23 on SyntheticRubbers.Current edition approved Nov. 1, 2003. Published December 2003. Originallyapproved in 1977. Last previous edition approved in 2002 as D 3568 98 (2002).2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Cu
14、stomer 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 mixer available from Hobart Corp., Troy, OH 45374, has been foundsatisfactory
15、for this purpose.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.“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 biconicalblende
16、r 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 recommended that a blend of carbon black and oilbe prep
17、ared 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 black and then gently whipping until uniformly blended. Le
18、t stand 24h and blend again before using.4EViscosity is 16.8 6 1.2 mm2/s at 100C in accordance with Test Method D 88and Practice D 2161. Viscosity gravity constant is 0.8896 0.002 in accordancewith Test Method D 2501. Available in 1 and 5-gal (3.8 and 19-dm3) quantities fromSun Oil Co. and is distri
19、buted 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 are available from ASTM Headquarters.GFor mill and in
20、ternal 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 blend to the nearest 0.01 g and individual compoundi
21、ngmaterial, 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 terpolymers withan ethylene content greater than appr
22、oximately 67 % by mass(which describes high green-strength extrusion grade rubbers).For determining ethylene content, refer to Test MethodsD 3900.4.1.3 Formula 3 shall apply to oil extended EPDM rubbers.5. Sample Preparation5.1 Obtain and prepare the test samples in accordance withPractice D 3896.6.
23、 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 characteristics of the EPDM rubber aresomewhat more di
24、fficult 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 carbon black dispersionwill be obtained by the mill
25、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 PracticeD 3182.6.2.2 Initial Mix Cycle:Dura-tion,minAccumu-lative,minAdjust the internal mixer temperature to achievethe discharge conditi
26、ons 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 the ram and clean the mixer throat andthe top of th
27、e 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 6 5C (122 6 9F) withan opening of 2.5 mm (0.10 in.
28、).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). Close the discharge gate, start the rotorsat 8 rad/s (
29、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, whichever occurs first. Discharge thebatch.1.5 max 2.0
30、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 D 1646 or vulcani-zation characteristics in accordance with TestMethod D 2084, or bo
31、th, 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, condition thesheeted compound for 1 to 24 h at 23 6 3C
32、(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 Mixer (MIM) Procedure:For general mixing procedur
33、e, refer to PracticeD 3182. Mix with the head temperature of theminiature internal mixer maintained at 60 6 3C(140 6 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 the temperatureset at 50 6 5C (122 6 9F) and an ope
34、ning 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 add the zinc oxide, sulfur,stearic acid, TMTD
35、, 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, remove the mixingchamber, and discharge the
36、 batch. Record the maximum batchtemperature indicated, if desired.D35680326.2.2.2 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 differs fromthe theoretical value by m
37、ore than 0.5 %, discard the batch.6.2.2.4 Cut a specimen for testing of vulcanization charac-teristics in accordance with Test Method D 2084 or D 5289 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 If either compounded viscosity or s
38、tress-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 Methods D 1646 if required.6.2.2.7 If ten
39、sile 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 effects of mill direction.Cool on a
40、 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 container to preventabsorption of moisture from the air, or
41、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 PracticeD 3182.6.3.2 Mixing Cycle:NOTE 2The indicated mill openings are desired and should bemaintained in so far as possible to provide a good rolling bank at the nipof th
42、e 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.)opening.1.0 1.0Add the mixture of zinc oxide, carbon
43、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 beenincorporated, make three34 cuts from each side.13.
44、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 set at 1.3 mm (0.05 in.) opening.3.0 17.0Make three34
45、 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 value by more than 0.5
46、%, discard the batch.6.3.2.2 Cut a specimen to allow testing of compoundviscosity in accordance with Test Methods D 1646, or D 6204,or vulcanization characteristics in accordance with TestMethod D 2084, or D 5289, if these are desired.6.3.2.3 If stress-strain testing is to be conducted, sheet offthe
47、 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 maximum p
48、reci-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 mixing procedure, refer to PracticeD 3182.6.4.2 Initial Mix
49、 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 the batch from the mill. Set the mill openingto 0.8 mm (0.032
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