1、Designation: D3185 06 (Reapproved 2010)Standard Test Methods forRubberEvaluation of SBR (Styrene-Butadiene Rubber)Including Mixtures With Oil1This standard is issued under the fixed designation D3185; the number immediately following the designation indicates the year oforiginal adoption or, in the
2、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 cover the standard materials, testformulas, mixing procedures, and te
3、st methods for 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 solut
4、ion SBR and solution 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
5、, 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:2D412 Test Methods for Vulcanized Rubber and Thermo-
6、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 MeterD3182 Practice for RubberMaterials, Equipment, andProcedures for Mixing St
7、andard Compounds and Prepar-ing Standard Vulcanized SheetsD3896 Practice for Rubber From Synthetic SourcesSamplingD4483 Practice for Evaluating Precision for Test MethodStandards in the Rubber and Carbon Black ManufacturingIndustriesD5289 Test Method for Rubber PropertyVulcanizationUsing Rotorless C
8、ure MetersD6204 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 Met
9、hods3.1 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 InternalMi
10、xer (MIM) 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 andde
11、velopment 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 recommend
12、ed that 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 a1These test methods are under the jurisdiction of ASTM Committee D11 onRubber and are the direct responsibility
13、 of Subcommittee D11.23 on SyntheticRubbers.Current edition approved Dec. 1, 2010. Published February 2011. Originallyapproved in 1973. Last previous edition approved in 2006 as D3185 06. DOI:10.1520/D3185-06R10.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Cus
14、tomer 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 International, 100 Barr Ha
15、rbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.proportional mass of each material in a dry powder blendersuch 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-pigmente
16、d, non-oil-extended rubber types. 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
17、.5.2 Standard Formulas for Oil Masterbatch 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 specifie
18、s Formula 1A for evaluation of general 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 pr
19、oportional massof each material in 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 PracticeD3896.7. Mixing Procedures7.1 Three mixing procedures are provid
20、ed:7.1.1 Method AMill mix (7.2).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 PracticeD3182.7.2.2 Mix with the mill
21、roll temperature maintained at 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 batc
22、h mass. If it differs from the theoretical value bymore than 0.5 %, discard the batch.TABLE 1 Standard Non-Oil Extended SBR Test FormulasMaterial IRM-SRM No. Quantity, Parts by Mass1A 2ASBR or masterbatch . 100.00 100.00Zinc oxideA3.00 3.00SulfurA1.75 1.75Stearic acidA1.00 1.00Oil furnace blackBA50.
23、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 been dried for1hat125 6 3C.CN-tert-butyl-2-benzothiazolesulfenamide.DFor mill batches,
24、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 to the nearest 0.1 g, thecompounding material blend to the nearest 0.01 g, and the indi
25、vidual 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 BaseMasterbatch 125.00 137.50 150.00 162.50 175.00 100 + YAZinc oxideB3.00 3.00 3.00 3
26、.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 194.50 213.38 232.25 251.13 270.00Batch factor for mill mixE2.4 2.2 2.0 1.9 1.7Batch fa
27、ctor 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 Black (IRB) which has been dried for 1 h at 125 6 3C.DN-tert-butyl-2-benzothiazolesulfenam
28、ide.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 rubber and carbon black to the nearest 0.1 g, the compounding material blend to the nea
29、rest 0.01 g and the individual compoundingmaterials, if used, to the nearest 0.001 g.D3185 06 (2010)27.2.3.2 If required, cut samples from the batch to allowtesting of compound viscosity and processability in accordancewith Test Methods D1646 or D6204, and vulcanization char-acteristics in accordanc
30、e with Test Methods D2084 or D5289.7.2.3.3 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 D3182.7.3 Method BMiniature Internal Mixer Procedure:7.3.1 For general mixing procedures refer
31、to PracticeD3182. Mix with the head 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
32、 0.5 mm (0.02 in.). Cut the sheet into 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 temperatureindic
33、ated, if desired.7.3.3.2 Immediately 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 mil
34、l six timeswith an opening of 0.8 mm (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
35、in accordancewith Test Methods D1646 or D6204, and vulcanization char-acteristics in accordance with Test Methods D2084 or D5289.7.3.3.5 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
36、3182.7.4 Method CInternal Mixer:7.4.1 For general mixing procedure refer to Practice D3182.7.4.2 Mixing Cycle-Initial MixSee Table 5.7.4.2.1 After mixing according to Table 5, measure andrecord the batch mass. If it differs from the theoretical value bymore than 0.5 %, discard the batch.TABLE 3 Mill
37、 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 the mill.Duration, min Accumulative, minSet the mill opening at 1.15 mm (0.045 in.) and band the rubber onthe slo
38、w 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 thestearic acid has been incorporated.211Add the carbon black evenly across the mill at a uniform rate. Whenabout ha
39、lf 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, openthe 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
40、(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.228Open the mill to give a minimum batch thickness of 6 mm (0.25 in.)and pass the stock through the mill four ti
41、mes, 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 the timer.00Masticate the rubber. 1.0 1.0Raise the ram and add all the zinc oxide, sulfur, stearic acid, andTBBS
42、 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 9.0D3185 06 (2010)37.4.2.2 Pass the batch immediately through the standardlaboratory mill three times, set at 6.0 mm (0.25 in.) and 4065
43、C (104 6 9F).7.4.2.3 Allow the batch to rest 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 allowtes
44、ting of compound viscosity and processability in accordancewith Test Methods D1646 or D6204, and vulcanization char-acteristics in accordance with Test Methods D2084 or D5289.7.4.3.3 If tensile stress strain tests are required, sheet off toa finished thickness of approximately 2.2 mm (0.087 in.) and
45、condition the compound according to Practice D3182.8. Testing Procedures8.1 For stress-strain testing, prepare the test sheets andvulcanize them in accordance with Practice D3182.8.1.1 The recommended standard vulcanization times forthe mill mixed compound are 25, 35, and 50 min at 145C(293F). The r
46、ecommended standard vulcanization time 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
47、operations;however, slightly different results may be obtained.8.1.3 Prepare test specimens and obtain tensile stress, ten-sile strength, and elongation in accordance with Test MethodsD412.8.2 An alternative to measuring vulcanization characteris-tics by means of tensile stress measurement on vulcan
48、izates isthe measurement of vulcanization characteristics in accordancewith Test Method D2084 (Oscillating Disk Cure MeterMethod) or Test Method D5289 (Rotorless Cure MeterMethod). These methods will not produce equal results.8.2.1 The recommended Test Method D2084 test conditionsare 1.67 Hz (100 cp
49、m) oscillation frequency, 1 oscillationamplitude, 160C die temperature, 30-min test time, and nopreheating. The recommended Test Method D5289 test condi-tions are 1.67 Hz (100 cpm) oscillation frequency, 0.5oscillation amplitude, 160C die temperature, 30-min test time,and no preheating. Test condition tolerances are specified bythe test methods.TABLE 5 Internal MixerInitial CycleDuration, min Accumulative, minAdjust the internal mixer temperature to achieve the dischargeconditions outlined below. Close the discharge gate, start
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