1、Designation: D 3185 06Standard Test Methods forRubberEvaluation of SBR (Styrene-Butadiene Rubber)Including Mixtures With Oil1This standard is issued under the fixed designation D 3185; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision
2、, 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 cover the standard materials, testformulas, mixing procedures, and test methods for
3、the evalu-ation of emulsion polybutadiene (EBR) and styrene-butadienerubbers (SBR) including the emulsion polybutadiene oil mas-terbatch rubbers, SBR oil masterbatches, and partiallycrosslinked and high Mooney rubbers.1.2 These test methods are also applicable to certain typesof solution SBR and sol
4、ution SBR oil masterbatches that areused in applications requiring vulcanization.1.3 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for informationonly.1.4 This standard does not purport to address all of thesafety concerns, if any, associated wi
5、th 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 412 Test Methods for Vulcanized Rubber and Thermo-plastic Elasto
6、mersTensionD 1646 Test Methods for RubberViscosity, Stress Relax-ation, and Pre-Vulcanization Characteristics (Mooney Vis-cometer)D 2084 Test Method for Rubber PropertyVulcanizationUsing Oscillating Disk Cure MeterD 3182 Practice for RubberMaterials, Equipment, andProcedures for Mixing Standard Comp
7、ounds and Prepar-ing Standard Vulcanized SheetsD 3896 Practice for Rubber From Synthetic SourcesSamplingD 4483 Practice for Evaluating Precision for Test MethodStandards in the Rubber and Carbon Black ManufacturingIndustriesD 5289 Test Method for Rubber PropertyVulcanizationUsing Rotorless Cure Mete
8、rsD 6204 Test Method for RubberMeasurement of Unvul-canized Rheological Properties Using Rotorless ShearRheometers2.2 ISO Standard:ISO 2322 Rubber, Styrene-Butadiene (SBR)Emulsion-Polymerized General-Purpose TypeTest Recipe andEvaluation of Vulcanization Characteristics33. Summary of Test Methods3.1
9、 These test methods include the standard test formulas,mixing procedures, and test methods for evaluating the follow-ing types of synthetic rubbers:3.1.1 Non-Oil-Extended Types, mill and Miniature InternalMixer (MIM) mixing procedures.3.1.2 Oil Masterbatch Types, mill and Miniature InternalMixer (MI
10、M) mixing procedures.3.2 No correlation between results for mill and MIM mixingprocedures is implied.4. Significance and Use4.1 These test methods are mainly intended for refereepurposes but may be used for quality control of syntheticrubber production. They may also be used in research anddevelopme
11、nt work and for comparison of different rubbersamples in a standard formula.4.2 These test methods may also be used to obtain values forcustomer acceptance of rubber.5. Standard Test Formulas5.1 Standard Formulas for Non-Oil-Extended TypesSeeTable 1.5.1.1 For the MIM procedure it is recommended that
12、 a blendof compounding materials, excluding carbon black, be pre-pared to improve accuracy in the weighing of these materials.The compounding material blend is prepared by blending aproportional mass of each material in a dry powder blender1These test methods are under the jurisdiction of ASTM Commi
13、ttee D11 onRubber and are the direct responsibility of Subcommittee D11.23 on SyntheticRubbers.Current edition approved March 1, 2006. Published March 2006. Originallyapproved in 1973. Last previous edition approved in 2005 as D 3185 05.2For referenced ASTM standards, visit the ASTM website, www.ast
14、m.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 American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036.1Copyright ASTM I
15、nternational, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.such as a biconical blender or vee blender. A mortar and pestlemay be used for blending small quantities.5.1.2 Formula 1A shall apply to the general-purpose non-pigmented, non-oil-extended rubber types.
16、 It is also specifiedin International Standard ISO 2322 for evaluation of generalpurpose, nonpigmented, non-oil-extended rubbers. Formula 2Ashall apply to the partially crosslinked and high-Mooneyrubber (90 ML 1 + 4 at 100C) for example, SBR 1009, 1018,and 1012 types.5.2 Standard Formulas for Oil Ma
17、sterbatch TypesSeeTable 2.5.2.1 Formulas 1B to 6B shall apply to the general purposenonpigmented oil-extended rubber types according to the oilcontent of the rubber. Formula 1A may be used as analternative to Formulas 1B to 6B. International Standard ISO2322 specifies Formula 1A for evaluation of ge
18、neral purpose,nonpigmented, oil-extended SBR.5.2.2 For the MIM procedure it is recommended that a blendof compounding materials, excluding carbon black, be pre-pared to improve accuracy in the weighing of these materials.The pigment blend is prepared by blending a proportional massof each material i
19、n a dry powder blender such as a biconicalblender or vee blender. A mortar and pestle may be used forblending small quantities.6. Sample Preparation6.1 Obtain the test samples in accordance with PracticeD 3896.7. Mixing Procedures7.1 Three mixing procedures are provided:7.1.1 Method AMill mix (7.2).
20、7.1.2 Method BMiniature internal mixer (MIM) mix(7.3).7.1.3 Method CInternal mixer mix (7.4).NOTE 1These mixing methods may not obtain comparable results.7.2 Method AMill Mix Procedure:7.2.1 For general mixing procedures refer to PracticeD 3182.7.2.2 Mix with the mill roll temperature maintained at
21、50 65C (122 6 9F). The indicated mill openings are desired andshould be maintained insofar as possible to provide uniformityin the breakdown of the rubber due to milling.7.2.3 Mixing CycleSee Table 3.7.2.3.1 After mixing according to Table 3, measure andrecord the batch mass. If it differs from the
22、theoretical value bymore than 0.5 %, discard the batch.7.2.3.2 If required, cut samples from the batch to allowtesting of compound viscosity and processability in accordanceTABLE 1 Standard Non-Oil Extended SBR Test FormulasMaterial IRM-SRM No. Quantity, Parts by Mass1A 2ASBR or masterbatch . 100.00
23、 100.00Zinc oxideA3.00 3.00SulfurA1.75 1.75Stearic acidA1.00 1.00Oil furnace blackBA50.00 35.00TBBSCA1.00 1.00Total 156.75 141.75Batch factor for mill mixDBatch factor for MIM mixE:3.0 3.3Cam headBanbury head0.470.410.490.46AUse Current IRM/SRM.BThe current Industry Reference Black (IRB), which has
24、been dried for1hat125 6 3C.CN-tert-butyl-2-benzothiazolesulfenamide.DFor mill batches, weigh the rubber and carbon black to the nearest 1.0 g, thesulfur and accelerator to the nearest 0.02 g, and the other compounding materialsto the nearest 0.1 g.EFor MIM batches, weigh the rubber and carbon black
25、to the nearest 0.1 g, thecompounding material blend to the nearest 0.01 g, and the individual compoundingmaterials, if used, to the nearest 0.001 g.TABLE 2 Standard Oil Masterbatch Type SBR Test FormulasMaterial IRM-SRMNo.Quantity, Parts by Mass1B 2B 3B 4B 5B 6BFormula No.Parts Oil25 37.5 50 62.5 75
26、 BaseMasterbatch 125.00 137.50 150.00 162.50 175.00 100 + YAZinc oxideB3.00 3.00 3.00 3.00 3.00 3.00SulfurB1.75 1.75 1.75 1.75 1.75 1.75Stearic acidB1.00 1.00 1.00 1.00 1.00 1.00Oil furnace blackCB62.50 68.75 75.00 81.25 87.50 50 (100 + Y)0.011TBBSD384 1.25 1.38 1.50 1.63 1.75 1 (100 + Y)0.011Total
27、194.50 213.38 232.25 251.13 270.00Batch factor for mill mixE2.4 2.2 2.0 1.9 1.7Batch factor for MIM mix:Cam headD0.37 0.34 0.31 0.29 0.27Banbury headF0.328 0.298 0.273 0.252 0.234AY = parts oil by mass per 100 parts base polymer in masterbatch.BUse Current IRM/SRM.CThe current Industry Reference Bla
28、ck (IRB) which has been dried for 1 h at 125 6 3C.DN-tert-butyl-2-benzothiazolesulfenamide.EFor mill batches, weigh the rubber and carbon black to the nearest 1.0 g, the sulfur and accelerator to the nearest 0.02 g, and the other compounding materials tothe nearest 0.1 g.FFor MIM batches, weigh the
29、rubber and carbon black to the nearest 0.1 g, the compounding material blend to the nearest 0.01 g and the individual compoundingmaterials, if used, to the nearest 0.001 g.D3185062with Test Methods D 1646 or D 6204, and vulcanizationcharacteristics in accordance with Test Methods D 2084 orD 5289.7.2
30、.3.3 If tensile stress strain tests are required, sheet off toa finished thickness of approximately 2.2 mm (0.087 in.) andcondition the compound according to Practice D 3182.7.3 Method BMiniature Internal Mixer Procedure:7.3.1 For general mixing procedures refer to PracticeD 3182. Mix with the head
31、temperature of the miniatureinternal mixer maintained at 60 6 3C (140 6 5F) and theunloaded rotor speed at 6.3 to 6.6 rad/s (60 to 63 rpm).7.3.2 Prepare the rubber by passing it through a mill onetime with the temperature set at 50 6 5C (122 6 9F) and anopening of 0.5 mm (0.02 in.). Cut the sheet in
32、to strips that areapproximately 25 mm (1 in.) wide, if desired.7.3.3 Mixing CycleSee Table 4.7.3.3.1 After mixing according to Table 4, turn off themotor, raise the ram, remove the mixing chamber, and dis-charge the batch. Record the maximum batch temperatureindicated, if desired.7.3.3.2 Immediately
33、 pass the discharge from the mixertwice through a standard mill maintained at 50 6 5C (122 69F) with a roll separation of 0.5 mm (0.020 in.) once, thentwice at a separation of 3 mm (0.12 in.) in order to dissipateheat. Pass the rolled batch endwise through the mill six timeswith an opening of 0.8 mm
34、 (0.31 in.) to enhance the dispersion.7.3.3.3 Measure and record the batch mass. If it differs fromthe theoretical value by more than 0.5 %, discard the batch.7.3.3.4 If required, cut samples from the batch to allowtesting of compound viscosity and processability in accordancewith Test Methods D 164
35、6 or D 6204, and vulcanizationcharacteristics in accordance with Test Methods D 2084 orD 5289.7.3.3.5 If tensile stress strain tests are required, sheet off toa finished thickness of approximately 2.2 mm (0.087 in.) andcondition the compound according to Practice D 3182.7.4 Method CInternal Mixer:7.
36、4.1 For general mixing procedure refer to PracticeD 3182.7.4.2 Mixing Cycle-Initial MixSee Table 5.TABLE 3 Mill Mixing CycleNOTEDo not cut any stock while free carbon black is evident in the bank or on the milling surface. Be certain to return to the milling stock anyingredients that drop through th
37、e mill.Duration, min Accumulative, minSet the mill opening at 1.15 mm (0.045 in.) and band the rubber onthe slow roll. Make34 cuts every12 min from alternate sides.77Add the sulfur slowly and evenly across the mill at a uniform rate. 2 9Add the stearic acid. Make one34 cut from each side after thest
38、earic acid has been incorporated.211Add the carbon black evenly across the mill at a uniform rate. Whenabout half the black is incorporated, open the mill to 1.25 mm (0.050in.) and make one34 cut from each side. Then add the remainder ofthe carbon black. When all the black has been incorporated, ope
39、nthe mill to 1.40 mm (0.055 in.) and make one34 cut from each side.10 21Add the other materials at the 1.40-mm (0.055-in.) setting. 3 24Make three34 cuts from each side and cut the batch from the mill. 2 26Set the rolls at 0.8 mm (0.032 in.). Pass the rolled batch endwisethrough the mill six times.2
40、28Open the mill to give a minimum batch thickness of 6 mm (0.25 in.)and pass the stock through the mill four times, folding it back on it-self each time.129TABLE 4 Miniature Internal Mixer CycleDuration, min Accumulative, minCharge the mixing chamber with the rubber strips, lower the ram,and start t
41、he timer.00Masticate the rubber. 1.0 1.0Raise the ram and add all the zinc oxide, sulfur, stearic acid, andTBBS that have been previously blended, taking care to avoid anyloss. Then add the carbon black, sweep the orifice, and lower theram.1.0 2.0Allow the batch to mix. 7.0 9.0D31850637.4.2.1 After
42、mixing according to Table 5, measure andrecord the batch mass. If it differs from the theoretical value bymore than 0.5 %, discard the batch.7.4.2.2 Pass the batch immediately through the standardlaboratory mill three times, set at 6.0 mm (0.25 in.) and 4065C (104 6 9F).7.4.2.3 Allow the batch to re
43、st for 1 to 24 h.7.4.3 Final MixSee Table 6.7.4.3.1 After mixing according to Table 6, measure andrecord the batch mass. If it differs from the theoretical value bymore than 0.5 %, discard the batch.7.4.3.2 If required, cut samples from the batch to allowtesting of compound viscosity and processabil
44、ity in accordancewith Test Methods D 1646 or D 6204, and vulcanizationcharacteristics in accordance with Test Methods D 2084 orD 5289.7.4.3.3 If tensile stress strain tests are required, sheet off toa finished thickness of approximately 2.2 mm (0.087 in.) andcondition the compound according to Pract
45、ice D 3182.8. Testing Procedures8.1 For stress-strain testing, prepare the test sheets andvulcanize them in accordance with Practice D 3182.8.1.1 The recommended standard vulcanization times forthe mill mixed compound are 25, 35, and 50 min at 145C(293F). The recommended standard vulcanization time
46、for theminiature internal mixer compound is 35 min at 145C.8.1.2 Condition the cured sheets for 16 to 96 h at atemperature of 23 6 3C (73 6 5F).NOTE 2Quality control of rubber production may require testingwithin 1 to6htoprovide close surveillance of the plant operations;however, slightly different
47、results may be obtained.8.1.3 Prepare test specimens and obtain tensile stress, ten-sile strength, and elongation in accordance with Test MethodsD 412.8.2 An alternative to measuring vulcanization characteris-tics by means of tensile stress measurement on vulcanizates isthe measurement of vulcanizat
48、ion characteristics in accordancewith Test Method D 2084 (Oscillating Disk Cure MeterMethod) or Test Method D 5289 (Rotorless Cure MeterMethod). These methods will not produce equal results.8.2.1 The recommended Test Method D 2084 test condi-tions are 1.67 Hz (100 cpm) oscillation frequency, 1 oscil
49、la-tion amplitude, 160C die temperature, 30-min test time, andno preheating. The recommended Test Method D 5289 testTABLE 5 Internal MixerInitial CycleDuration, min Accumulative, minAdjust the internal mixer temperature to achieve the dischargeconditions outlined below. Close the discharge gate, start the rotorat 8.1 rad/s (77 rpm) and raise the ram.0.5 0.5Charge one half the rubber, all of the zinc oxide, carbon black,stearic acid, and then the other one half of the rubber. Lower theram.3.0 3.5Allow the batch to mix. 0.5 4.0Raise t
