1、Designation: D3484 06 (Reapproved 2016)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 Thermoplas-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, a
6、nd Pro-cedures for Mixing Standard 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 PropertyVulc
7、anizationUsing Rotorless Cure MetersD6204 Test Method for RubberMeasurement of Unvulca-nized Rheological Properties Using Rotorless Shear Rhe-ometers2.2 ISO Standard:ISO 2476 Rubber, Butadiene (BR) Solution PolymerizedTypesTest Recipe and Evaluation Characteristics33. Significance and Use3.1 These t
8、ests 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
9、 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 24
10、76 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 M
11、ixer/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 somew
12、hat more difficult than that of other rubbers the1These test methods are under the jurisdiction 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 1976. Last pre
13、vious edition approved in 2010 as D3484 06 (2010). DOI:10.1520/D3484-06R16.2For referenced ASTM 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
14、 ASTM website.3Available from American National Standards Institute, 25 W. 43rd St., 4thFloor, New York, NY 10036.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1use of one of the internal mixer procedures is recommended (Method A,B,
15、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):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.TABLE 1 Standard
22、 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 mixE4.0 0.036 Y 4.0Ba
23、tch 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 100 parts base po
24、lymer 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, and theother compoun
25、ding 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 a blend of compoun
26、ding 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 beused for blendin
27、g 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 the rubber, all o
28、f 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) or a total of 6 min
29、 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 5C (104 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 r
30、am.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 5C (230 9F) or a total mixing timeof 3 min is reach
31、ed, whichever occurs first.Discharge the batch.2.5 3.0With the rolls of a standard laboratory millmaintained at 70 5C (158 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 t
32、he compoundthrough four times, folding it back on itselfeach time.1.0 6.0D3484 06 (2016)26.4.2 Mill Mixing 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.6.4.2.2 If required,
33、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 thickness o
34、f 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 theunloaded
35、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 25 mm(1 in.)
36、 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 mixertwice th
37、rough 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 thedispersion.6.5.
38、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 char-acterist
39、ics 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-strain testing,
40、prepare the test sheets andvulcanize them in accordance with Practice D3182.TABLE 4 Mill Final Mixing CycleDuration,minAccumulative,minSet the mill opening at 1.50 mm (0.059 in.)and temperature at 40 5C (104 9F),band the masterbatch on the slow roll.00Add the TBBS accelerator, taking care toavoid an
41、y loss. Sweep the mill 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 en
42、dwise 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.19TABLE 5 Mill Mixing CycleNOTE 1Do not cut any stock while free carbon black is evident in the bank or on the mill
43、ing surface. Be certain to return any materials that dropthrough the mill to the milling stock.Duration,minAccumulative,minWith the mill roll temperature set at 40 5C (104 9F) and the opening at 1.20 mm (0.047 in.),band the rubber on the slow roll.00Add the zinc oxide evenly across the rolls. Make t
44、wo34 cuts from each side. 2 2Add one-half of the carbon black evenly across the mill at a uniform rate. Make two34 cuts on eachside and then add the stearic acid evenly across the rolls. Continue to make34 cuts from each sideas necessary during the remaining time.10 12Open the rolls to 1.80 mm (0.07
45、1 in.) and add the remaining carbon black evenly across the rolls,making sure all materials in the pan are added to the batch. Make two34 cuts from each side.12 to 16 24 to 28Add the TBBS accelerator and sulfur, taking care to avoid any loss. Sweep the mill pan and add untilall ingredients are in th
46、e batch.2 26to30Make three34 cuts from each side. 2 28to32Cut the stock from the mill. Set the opening at 0.8 mm (0.032 in.). Pass the rolled stock endwisethrough the mill six times.2 30to34Open the mill to give a minimum stock thickness of 6 mm (0.25 in.) and pass the compound throughthe mill four
47、times, folding it back on itself each time.1 31to35D3484 06 (2016)37.1.1 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 at
48、 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 test
49、 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 accordancewith 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
