1、Designation: D 3484 06Standard Test Methods forRubberEvaluation of Oil-Extended Solution BR(Polybutadiene Rubber)1This standard is issued under the fixed designation D 3484; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year
2、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 the evalu-a
3、tion 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 of thesafety c
4、oncerns, 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:2D 412 Test Methods for Vulcanized Ru
5、bber and Thermo-plastic ElastomersTensionD 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, andProce
6、dures for Mixing Standard Compounds 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 PropertyVulcaniz
7、ationUsing Rotorless Cure MetersD 6204 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 tests
8、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 acceptance of r
9、ubber.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 2476 fo
10、r oil extended BR.5. Sample Preparation5.1 For test intended for referee purposes obtain and preparethe test samples in accordance with Practice D 3896.6. 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 Mixer
11、/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 somewhat
12、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.6.2 Internal Mixer Initial Mix (Methods A, B):1These test methods are under the jur
13、isdiction of ASTM Committee D11 onRubber and are the direct responsibility of Subcommittee D11.23 on SyntheticRubbers.Current edition approved Oct. 1, 2006. Published November 2006. Originallyapproved in 1976. Last previous edition approved in 2002 as D 3484 97 (2002).2For referenced ASTM standards,
14、 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, 25 W. 43rd St., 4thFloor, New York, N
15、Y 10036.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.6.2.1 For general mixing procedure refer to PracticeD 3182.6.2.2 Internal Mixer Initial MixSee Table 2.6.2.2.1 After mixing according to Table 2, measure andrecord the batch mas
16、s. 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 rest for 1 to 24 h.6.2.3
17、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 viscosity and processa
18、bility in accordancewith Test Methods D 1646 or D 6204, and vulcanizationcharacteristics in accordance with Test Methods D 2084 orD 5289.6.2.3.3 If tensile stress strain tests are required, sheet off toa finished thickness of approximately 2.2 mm (0.087 in.) andcondition the compound according to Pr
19、actice D 3182.6.3 Mixing Cycle for Final Mill Mix after Internal MixerInitial Mix (Method B):6.3.1 For general mixing procedures, refer to PracticeD 3182.6.3.2 Mixing Cycle for Mill Final Mix (Method B)SeeTable 4.6.3.2.1 After mixing according to Table 4, measure andrecord the batch mass. If it diff
20、ers 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 D 1646 or D 6204, and vulcanizationcharacteristics in accordance with Test Methods D 2084 orD 52
21、89.6.3.2.3 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 D 3182.6.4 Mill Mixing (Method C):6.4.1 For general mixing procedure, refer to PracticeD 3182.6.4.2 Mill Mixing CycleSee Table
22、5.TABLE 1 Standard BR Test FormulasMaterial IRM-SRM No.AQuantity, Parts by MassFormula No. 1 2OE-BR . 100.00 + YB100.00Zinc oxideA3.00 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 mix
23、E4.0 0.036 Y 4.0Batch Factor for InternalMixerE1170 (1.020 + 0.00044Y)/total formulaparts7.7Batch Factor for MIM Mix(Formula 1)F70 (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
24、 100 parts base polymer in masterbatch.CThe current Industry Reference Black (IRB) shall be used.DTBBS is N-tert-butyl-2-benzothiazolesulfenamide.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, an
25、d theother compounding materials to the nearest 0.1 g.FFor MIM mixes, weigh the rubber and carbon black 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. For the MIM procedure, it is recom-mended that
26、a blend of compounding materials, excluding carbon black, beprepared to improve the accuracy of the weighing of these materials. 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
27、beused for blending small quantities.TABLE 2 Internal Mixer - Initial CycleDuration,minAccumulative,minAdjust the internal mixer 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
28、 the rubber, all of the zincoxide, carbon black, stearic acid, and thenthe other one-half of the rubber. Lower theram.0.5 0.5Allow 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) o
29、r a total of 6 min is reached,whichever occurs first. Discharge the batch.2.0 6.0TABLE 3 Internal Mixer - Final CycleDuration,minAccumulative,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/
30、min), and raise the ram.0.0 0.0Charge one-half of the batch, with all thesulfur and accelerator rolled into this portionof the batch 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 mix
31、ing timeof 3 min is reached, whichever occurs first.Discharge the batch.2.5 3.0With the rolls of a standard laboratory millmaintained 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
32、 of6 mm (0.25 in.) and pass the compoundthrough four times, folding it back on itselfeach time.1.0 6.0D34840626.4.2.1 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.6.4.2.2 If required, cut samples fr
33、om the batch to allowtesting of compound viscosity and processability in accordancewith Test Methods D 1646 or D 6204, and vulcanizationcharacteristics in accordance with Test Methods D 2084 orD 5289.6.4.2.3 If tensile stress strain tests are required, sheet off toa finished thickness of approximate
34、ly 2.2 mm (0.087 in.) andcondition the compound according to Practice D 3182.6.5 Miniature Internal Mixer (Method D):6.5.1 For general mixing procedures, refer to PracticeD 3182. Mix with the head temperature of the miniatureinternal mixer maintained at 60 6 3C (140 6 5F) and theunloaded rotor speed
35、 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 25 mm(1 in.) wide, if d
36、esired.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 mixertwice through a sta
37、ndard 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 thedispersion.6.5.3.3 Measure
38、 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 D 1646 or D 6204, and vulcanizationcharacteristics in acco
39、rdance with Test Methods D 2084 orD 5289.6.5.3.5 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 D 3182.7. Preparation and Testing of Vulcanizates7.1 For stress-strain testing, prepare t
40、he test sheets andvulcanize them in accordance with Practice D 3182.7.1.1 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 D(MIM) is 35 min a
41、t 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 obtained.7.1.3 Prepare tes
42、t specimens and obtain the tensile stress,tension, and elongation in accordance with Test MethodsD 412.7.2 An alternative to measuring vulcanization characteris-tics by means of tensile stress measurement on vulcanizates isthe measurement of vulcanization characteristics in accordancewith Test Metho
43、d D 2084 (Oscillating Disk Cure MeterMethod) or Test Method D 5289 (Rotorless Cure MeterMethod). These methods will not produce equal results.7.2.1 The recommended Test Method D 2084 test condi-tions are 1.67 Hz (100 cpm) oscillation frequency, 1 oscilla-tion amplitude, 160C die temperature, 30-min
44、test time, andno preheating. The recommended Test Method D 5289 testconditions 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 standard te
45、st 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 D 4483. Refer to this practice for terminology andother statistical calculation details.8.2 The precision r
46、esults 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 that the par
47、ameters 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 test4Supporting data have been filed at ASTM International Headquarters and maybe obt
48、ained 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
49、pan and adduntil all the accelerator is in the batch. Makethree34 cuts from each side.33Add the sulfur and that which falls into themill pan. Make one34 cut from each side.36Cut the batch from the mill and set the millroll opening at 0.8 mm (0.032 in.). Pass therolled stock endwise through the mill sixtimes.28Open the mill to give a minimum stockthickness of 6 mm (0.25 in.) and pass thecompound through the mill four times, foldingit back on itself each time.19D3484063run included weighing of ingredients, preparation of mill m
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