1、Designation: D3484 06 (Reapproved 2010)Standard Test Methods forRubberEvaluation of Oil-Extended Solution BR(Polybutadiene Rubber)1This standard is issued under the fixed designation D3484; the number immediately following the designation indicates the year oforiginal adoption or, in the case of rev
2、ision, 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 test methods
3、for the evalu-ation and production control of oil-extended polybutadienerubber (OE-BR) polymerized in an appropriate solution.1.2 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for informationonly.1.3 This standard does not purport to address all
4、 of thesafety concerns, 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:2D412 Test Methods for
5、 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 MeterD3182 Practice for RubberMaterials, Equipmen
6、t, andProcedures for Mixing Standard 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 Property
7、VulcanizationUsing Rotorless Cure MetersD6204 Test Method for RubberMeasurement of Unvul-canized Rheological Properties Using Rotorless ShearRheometers2.2 ISO Standard:ISO 2476 Rubber, Butadiene (BR) Solution PolymerizedTypesTest Recipe and Evaluation Characteristics33. Significance and Use3.1 These
8、 tests are mainly intended for referee purposes butmay also be used for quality control of rubber production. Theymay be used in research and development work for comparisonof different rubber samples in a standard formula.3.2 These test methods may also be used to obtain values forcustomer acceptan
9、ce of rubber.4. Standard Test Formulas4.1 Standard FormulasSee Table 1.4.2 Formula 1 is written based on 100 parts of rubber whileFormula 2 is written on the basis of 100 parts of themasterbatch. Either formula may be used, but these will notgive the same results.NOTE 1Formula 2 is specified in ISO
10、2476 for oil extended BR.5. Sample Preparation5.1 For test intended for referee purposes obtain and preparethe test samples in accordance with Practice D3896.6. Mixing Procedures6.1 The following four mixing test methods are offered:6.1.1 Method AInternal Mixer Procedure (6.2),6.1.2 Method BInternal
11、 Mixer/Mill Procedure (6.3),6.1.3 Method CMill Procedure (6.4), and6.1.4 Method DMiniature Internal Mixer Procedure (6.5).NOTE 2It is not implied that comparable results will be obtained bythese test methods.NOTE 3Since the mill handling characteristics of the solution polyb-utadiene rubbers are som
12、ewhat more difficult than that of other rubbers theuse of one of the internal mixer procedures is recommended (Method A,B, or D). The mill procedure (Method C) may be used provided a goodcarbon black dispersion is obtained.1These test methods are under the jurisdiction of ASTM Committee D11 onRubber
13、 and are the direct responsibility of Subcommittee D11.23 on SyntheticRubbers.Current edition approved Dec. 1, 2010. Published February 2011. Originallyapproved in 1976. Last previous edition approved in 2006 as D3484 06. DOI:10.1520/D3484-06R10.2For referenced ASTM standards, visit the ASTM website
14、, 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, 25 W. 43rd St., 4thFloor, New York, NY 10036.1Copyright ASTM
15、 International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.6.2 Internal Mixer Initial Mix (Methods A, B):6.2.1 For general mixing procedure refer to Practice D3182.6.2.2 Internal Mixer Initial MixSee Table 2.6.2.2.1 After mixing according to Table 2, measure
16、andrecord the batch mass. If it differs from the theoretical value bymore than 0.5 %, discard the batch.6.2.2.2 Pass the batch immediately through the standardlaboratory mill three times, with a mill opening of 6.0 mm(0.25 in.) and roll temperature of 70 6 5C (158 6 9F).6.2.2.3 Allow the batch to re
17、st for 1 to 24 h.6.2.3 Internal Mixer Final Mix (Method A)See Table 3.6.2.3.1 After mixing according to Table 3, measure andrecord the batch mass. If it differs from the theoretical value bymore than 0.5 %, discard the batch.6.2.3.2 If required, cut samples from the batch to allowtesting of compound
18、 viscosity and processability in accordancewith Test Methods D1646 or D6204, and vulcanization char-acteristics in accordance with Test Methods D2084 or D5289.6.2.3.3 If tensile stress strain tests are required, sheet off toa finished thickness of approximately 2.2 mm (0.087 in.) andcondition the co
19、mpound according to Practice D3182.6.3 Mixing Cycle for Final Mill Mix after Internal MixerInitial Mix (Method B):6.3.1 For general mixing procedures, refer to PracticeD3182.6.3.2 Mixing Cycle for Mill Final Mix (Method B)SeeTable 4.6.3.2.1 After mixing according to Table 4, measure andrecord the ba
20、tch mass. If it differs from the theoretical value bymore than 0.5 %, discard the batch.6.3.2.2 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 M
21、ethods D2084 or D5289.6.3.2.3 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 D3182.6.4 Mill Mixing (Method C):6.4.1 For general mixing procedure, refer to PracticeD3182.6.4.2 Mill Mixin
22、g CycleSee Table 5.6.4.2.1 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 1 Standard BR Test FormulasMaterial IRM-SRM No.AQuantity, Parts by MassFormula No. 1 2OE-BR . 100.00 + YB100.00Zinc oxid
23、eA3.00 3.00SulfurA1.50 1.50Stearic acidA2.00 2.00Oil furnace blackCA60.00 (100 + Y) 0.01 60.00TBBSDA0.90 (100 + Y) 0.01 0.90Total 167.40 + Y 167.40Batch factor for mill mixE4.0 0.036 Y 4.0Batch Factor for InternalMixerE1170 (1.020 + 0.00044Y)/total formulaparts7.7Batch Factor for MIM Mix(Formula 1)F
24、70 (1.020 + 0.00044Y)/total formulapartsBatch Factor for MIM Mix(Cam Head)F0.44Batch Factor for MIM Mix(Banbury Head)F0.38AUse current IRM/SRM.BY = parts of oil by mass per 100 parts base polymer in masterbatch.CThe current Industry Reference Black (IRB) shall be used.DTBBS is N-tert-butyl-2-benzoth
25、iazolesulfenamide.EFor mill and internal mixer batches, weigh the rubber and carbon black to thenearest 1.0 g, the sulfur and the TBBS accelerator to the nearest 0.02 g, and theother compounding materials to the nearest 0.1 g.FFor MIM mixes, weigh the rubber and carbon black to the nearest 0.1 g, th
26、ecompounding material blend to the nearest 0.01 g, and the individual compoundingmaterials, if used, to the nearest 0.001 g. For the MIM procedure, it is recom-mended that a blend of compounding materials, excluding carbon black, beprepared to improve the accuracy of the weighing of these materials.
27、 This materialblend is prepared by blending a proportional mass of each material in a dry powderblender such as a biconical blender or vee blender. A mortar and pestle may beused for blending small quantities.TABLE 2 Internal Mixer - Initial CycleDuration,minAccumulative,minAdjust the internal mixer
28、 temperature toachieve the discharge conditions outlinedbelow. Close the discharge gate, start therotors at 8.1 rad/s (77 r/min), and raise theram.0.0 0.0Charge one-half of the rubber, all of the zincoxide, carbon black, stearic acid, and thenthe other one-half of the rubber. Lower theram.0.5 0.5All
29、ow the batch to mix. 3.0 3.5Raise the ram, and clean the mixer throatand the top of the ram. Lower the ram.0.5 4.0Allow the batch to mix until a temperature of170C (338F) or a total of 6 min is reached,whichever occurs first. Discharge the batch.2.0 6.0TABLE 3 Internal Mixer - Final CycleDuration,mi
30、nAccumulative,minAdjust the internal mixer temperature to 40 65C (104 6 9F), turn off steam and turn onfull cooling water to the rotors, start the rotorsat 8.1 rad/s (77 r/min), and raise the ram.0.0 0.0Charge one-half of the batch, with all thesulfur and accelerator rolled into this portionof the b
31、atch before feeding to the mixer. Addthe remaining portion of the batch. Lower theram.0.5 0.5Allow the batch to mix until a temperature of110 6 5C (230 6 9F) or a total mixing timeof 3 min is reached, whichever occurs first.Discharge the batch.2.5 3.0With the rolls of a standard laboratory millmaint
32、ained at 70 6 5C (158 6 9F), and setat 0.8 mm (0.032 in.) opening, pass the rolledbatch endwise through the mill six times.2.0 5.0Open the rolls to give a minimum thickness of6 mm (0.25 in.) and pass the compoundthrough four times, folding it back on itselfeach time.1.0 6.0D3484 06 (2010)26.4.2.2 If
33、 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 D5289.6.4.2.3 If tensile stress strain tests are required, sheet off toa finished
34、thickness of approximately 2.2 mm (0.087 in.) andcondition the compound according to Practice D3182.6.5 Miniature Internal Mixer (Method D):6.5.1 For general mixing procedures, refer to PracticeD3182. Mix with the head temperature of the miniatureinternal mixer maintained at 60 6 3C (140 6 5F) and t
35、heunloaded rotor speed set at 6.3 to 6.6 rad/s (60 to 63 r/min).6.5.2 Prepare the rubber by passing through a mill one timewith the roll temperature set at 40 6 5C (104 6 9F) and anopening that will give a sheet approximately 0.5 mm (0.02 in.)thick. Cut the sheet into strips that are approximately 2
36、5 mm(1 in.) wide, if desired.6.5.3 MIM Mixing CycleSee Table 6.6.5.3.1 After mixing according to Table 6, turn off themotor, raise the ram, remove the mixing chamber and dis-charge the batch. Record the maximum batch temperatureindicated, if desired.6.5.3.2 Immediately pass the discharge from the mi
37、xertwice through a standard mill maintained at 40 6 5C (104 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 (0.032 in.) to enhance thedisp
38、ersion.6.5.3.3 Measure and record the batch mass. If it differs fromthe theoretical value by more than 0.5 %, discard the batch.6.5.3.4 If required, cut samples from the batch to allowtesting of compound viscosity and processability in accordancewith Test Methods D1646 or D6204, and vulcanization ch
39、ar-acteristics in accordance with Test Methods D2084 or D5289.6.5.3.5 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 D3182.7. Preparation and Testing of Vulcanizates7.1 For stress-strai
40、n testing, prepare the test sheets andvulcanize them in accordance with Practice D3182.7.1.1 The recommended standard vulcanization times forthe compounds prepared by Methods A, B, and C are 25, 35,and 50 min at 145C (293F). The recommended standardvulcanization time for compounds prepared by Method
41、 D(MIM) is 35 min at 145C (293F).7.1.2 Condition the cured sheets for 16 to 96 h at atemperature of 23 6 2C (73.4 6 3.6F).NOTE 4Quality control of rubber production may require testingwithin 1 to6htoprovide close surveillance of the plant operations,however, slightly different results may be obtaine
42、d.7.1.3 Prepare test specimens and obtain the tensile stress,tension, and elongation in accordance with Test MethodsD412.7.2 An alternative to measuring vulcanization characteris-tics by means of tensile stress measurement on vulcanizates isthe measurement of vulcanization characteristics in accorda
43、ncewith Test Method D2084 (Oscillating Disk Cure MeterMethod) or Test Method D5289 (Rotorless Cure MeterMethod). These methods will not produce equal results.7.2.1 The recommended Test Method D2084 test conditionsare 1.67 Hz (100 cpm) oscillation frequency, 1 oscillationamplitude, 160C die temperatu
44、re, 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.7.2.2 The recommended
45、 standard test parameters are ML,MH,tS1, t850 and t890.8. Precision and Bias48.1 The precision and bias section deals with test resultsobtained in an interlaboratory program organized according toPractice D4483. Refer to this practice for terminology andother statistical calculation details.8.2 The
46、precision results in this section give an estimate ofthe precision of this method with the materials used in theparticular interlaboratory test program as described below. Theprecision parameters should not be used for acceptance orrejection testing of any group of materials without documen-tation t
47、hat the parameters are applicable to the group ofmaterials and the specific testing protocols of the test method.8.3 A Class 3, Type 2 interlaboratory test program wasconducted in 1996 with ten participating laboratories. One testrun included weighing of ingredients, preparation of mill mixes(compou
48、nds), testing of compound Mooney viscosities, curemeter testing of compounds, vulcanization of compounds andstress/strain testing of the vulcanizates. Cure meter testing wasconducted at 160C (320F) and 1.7 Hz (100 cpm) with a 1arc for the oscillating disk cure meter and a 0.5 arc for therotorless cu
49、re meter. All ingredients were distributed by one4Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR: D11-1087.TABLE 4 Mill Final Mixing CycleDuration,minAccumulative,minSet the mill opening at 1.50 mm (0.059 in.)and temperature at 40 6 5C (104 6 9F),band the masterbatch on the slow roll.00Add the TBBS accelerator, taking care toavoid any loss. Sweep the mill pan and adduntil all the accelerator is in the batch. Makethree34 cuts from each side.33Add the s
