1、Designation: D3185 06 (Reapproved 2016)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 partially cross-linked and high Mooney rubbers.1.2 These test methods are also applicable to certain typesof sol
4、ution 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 a
5、ny, 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 Therm
6、oplas-tic ElastomersTensionD1646 Test Methods for RubberViscosity, StressRelaxation, and Pre-Vulcanization Characteristics(Mooney Viscometer)D2084 Test Method for Rubber PropertyVulcanizationUsing Oscillating Disk Cure MeterD3182 Practice for RubberMaterials, Equipment, and Pro-cedures for Mixing St
7、andard Compounds and PreparingStandard 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 Cur
8、e MetersD6204 Test Method for RubberMeasurement of Unvulca-nized Rheological Properties Using Rotorless Shear Rhe-ometers2.2 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 1.1These test methods are under the jurisdict
12、ion of ASTM Committee D11 onRubber and are the direct responsibility of Subcommittee D11.23 on SyntheticRubbers.Current edition approved June 1, 2016. Published July 2016. Originally approvedin 1973. Last previous edition approved in 2010 as D3185 06 (2010). DOI:10.1520/D3185-06R16.2For referenced A
13、STM 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.3Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4
14、th Floor, New York, NY 10036.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States15.1.1 For the MIM procedure it is recommended that a blendof compounding materials, excluding carbon black, be pre-pared to improve accuracy in the weighing
15、of these materials.The compounding material blend is prepared by blending aproportional 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-purposenonpigmente
16、d, non-oil-extended rubber types. It is also speci-fied in International Standard ISO 2322 for evaluation ofgeneral purpose, nonpigmented, non-oil-extended rubbers.Formula 2A shall apply to the partially crosslinked andhigh-Mooney rubber (90 ML 1 + 4 at 100C) for example,SBR 1009, 1018, and 1012 typ
17、es.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 specif
18、ies 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
19、proportional 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 prov
20、ided: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 mi
21、ll roll temperature maintained at 50 65C (122 6 9F). The indicated mill openings are desired andTABLE 1 Standard Non-Oil Extended SBR Test FormulasMaterial IRM-SRMNo.Quantity, Parts by Mass1A 2ASBR or masterbatch . 100.00 100.00Zinc oxideA3.00 3.00SulfurA1.75 1.75Stearic acidA1.00 1.00Oil furnace bl
22、ackBA50.00 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 for 1 h at 125 3C.CN-tert-butyl-2-benzothiazolesulfenamide.DFor mill
23、 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 to the nearest 0.1 g, thecompounding material blend to the nearest 0.01 g, an
24、d 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 BaseMasterbatch 125.00 137.50 150.00 162.50 175.00 100 + YAZinc oxideB3.00 3
25、.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 194.50 213.38 232.25 251.13 270.00Batch factor for mill mixE2.4 2.2 2.0 1.9 1
26、.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 Black (IRB) which has been dried for 1 h at 125 3C.DN-tert-butyl-2-benzothiazole
27、sulfenamide.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 to thenearest 0.1 g.FFor MIM batches, weigh the rubber and carbon black to the nearest 0.1 g, the compounding material blend to
28、 the nearest 0.01 g and the individual compoundingmaterials, if used, to the nearest 0.001 g.D3185 06 (2016)2should 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 an
29、drecord the batch mass. If it differs from the 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 accordancewith Test Methods D1646 or D6204, and vulcanization char-acteristics in accordan
30、ce 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 o
32、f 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 temperatureindi
33、cated, 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 mi
34、ll 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
36、D3182.7.4 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.7.4.2.2 Pas
37、s 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 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 theoreti
38、cal 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 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
39、stress strain tests are required, sheet off toa finished thickness of approximately 2.2 mm (0.087 in.) andcondition the compound according to Practice D3182.8. Testing Procedures8.1 For stress-strain testing, prepare the test sheets andvulcanize them in accordance with Practice D3182.8.1.1 The recom
40、mended standard vulcanization times forthe mill mixed compound are 25, 35, and 50 min at 145CTABLE 3 Mill Mixing CycleNOTE 1Do 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 mi
41、ll.Duration, min Accumulative, minSet the mill opening at 1.15 mm (0.045 in.) and band the rubber on the slow roll. Make34cuts 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 the stear
42、ic acid has been incor-porated.211Add the carbon black evenly across the mill at a uniform rate. When about half the black isincorporated, open the mill to 1.25 mm (0.050 in.) and make one34 cut from each side.Then add the remainder of the carbon black. When all the black has been incorporated,open
43、the 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 endwise through the mill six times.
44、2 28Open the mill to give a minimum batch thickness of 6 mm (0.25 in.) and pass the stockthrough the mill four times, folding it back on itself each time.129D3185 06 (2016)3(293F). The recommended standard vulcanization time for theminiature internal mixer compound is 35 min at 145C.8.1.2 Condition
45、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 results may be obtained.8.1.3 Prepare test specimens and obtain tensile str
46、ess, ten-sile strength, and elongation in accordance with Test MethodsD412.TABLE 4 Miniature Internal Mixer CycleDuration, min Accumulative, minCharge the mixing chamber with the rubberstrips, lower the ram, and start the timer.00Masticate the rubber. 1.0 1.0Raise the ram and add all the zinc oxide,
47、sulfur, stearic acid, and TBBS that have beenpreviously blended, taking care to avoid anyloss. Then add the carbon black, sweep theorifice, and lower the ram.1.0 2.0Allow the batch to mix. 7.0 9.0TABLE 5 Internal MixerInitial CycleDuration, min Accumulative, minAdjust the internal mixer temperature
48、toachieve the discharge conditions outlinedbelow. Close the discharge gate, start therotor at 8.1 rad/s (77 rpm) and raise the ram.0.5 0.5Charge one half the rubber, all of the zincoxide, carbon black, stearic acid, and then theother one half of the rubber. Lower the ram.3.0 3.5Allow the batch to mi
49、x. 0.5 4.0Raise the ram and clean the mixer throat andthe top of the ram. Lower the ram.2.0 6.0Allow the batch to mix until a temperature of170C (338F) or a total mixing time of 6 minis reached, whichever occurs first. Dischargethe batch.2.0 6.0TABLE 6 Internal MixerFinal CycleDuration, min Accumulative, minAdjust the internal mixer temperature to 40 5C (104 9F), turn off steam and turn on fullcooling water to the rotors, at 8.1 rad/s (77rpm), and raise the ram.00Charge12 the batch, with all the sulfur andaccelerator ro
