1、Designation: D3189 06 (Reapproved 2011)Standard Test Methods forRubberEvaluation of Solution BR (Polybutadiene Rubber)1This standard is issued under the fixed designation D3189; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the y
2、ear 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, testformula, mixing procedures, and test methods for evaluatio
3、n ofbutadiene rubber (BR) made by polymerization in solution.1.2 The values stated in SI units are to be regarded as thestandard. The values in parentheses are for information only.1.3 This standard does not purport to address the safetyconcerns, if any, associated with its use. It is the responsibi
4、lityof the user of this standard to establish appropriate safety andhealth practices and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D88 Test Method for Saybolt ViscosityD412 Test Methods for Vulcanized Rubber and Thermo-plastic Elasto
5、mersTensionD1646 Test Methods for RubberViscosity, Stress Relax-ation, and Pre-Vulcanization Characteristics (Mooney Vis-cometer)D2084 Test Method for Rubber PropertyVulcanizationUsing Oscillating Disk Cure MeterD2161 Practice for Conversion of Kinematic Viscosity toSaybolt Universal Viscosity or to
6、 Saybolt Furol ViscosityD2501 Test Method for Calculation of Viscosity-GravityConstant (VGC) of Petroleum OilsD3040 Practice for Preparing Precision Statements for Stan-dards Related to Rubber and Rubber Testing3D3182 Practice for RubberMaterials, Equipment, andProcedures for Mixing Standard Compoun
7、ds 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 Cure MetersD620
8、4 Test Method for RubberMeasurement of Unvul-canized Rheological Properties Using Rotorless ShearRheometersNOTE 1The specific dated edition of Practice D3040 that prevails inthese test methods is referenced in the precision section.3. Significance and Use3.1 These test methods are intended mainly fo
9、r refereepurposes but may be used for quality control of rubberproduction. They may also be used in research and develop-ment work and for comparison of different rubber samples in astandard formula.3.2 These tests may be used to obtain values for customeracceptance of rubber.4. Standard Test Formul
10、a4.1 Standard FormulasSee Table 1.5. Sample Preparation5.1 For tests intended for referee purposes obtain andprepare the test samples in accordance with Practice D3896.6. Mixing Procedures6.1 The following four mixing procedures are offered:6.1.1 Test Method AInternal Mixer for Initial and FinalMix,
11、6.1.2 Test Method BInternal Mixer Initial Mix with FinalMill Mix,6.1.3 Test Method CMill Mix, and6.1.4 Test Method DMiniature Internal Mixer Mix.NOTE 2The compound may be prepared either on a mill or in aninternal mixer or in a miniature internal mixer although slightly differentresults may be obtai
12、ned.NOTE 3Since the mill handling characteristics of the solution polyb-utadiene rubber are somewhat more difficult than for other polymers; theuse of one of the internal mixer procedures is recommended (Test Method1These test methods are under the jurisdiction of ASTM Committee D11 onRubber and are
13、 the direct responsibility of Subcommittee D11.23 on SyntheticRubbers.Current edition approved Nov. 1, 2011. Published January 2012. Originallyapproved in 1973. Last previous edition approved in 2006 as D3189 06. DOI:10.1520/D3189-06R11.2For referenced ASTM standards, visit the ASTM website, www.ast
14、m.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.3Withdrawn. The last approved version of this historical standard is referencedon www.astm.org.1Copyright ASTM International
15、, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.A, B, or D). The mill procedure (Test Method C) may be used providedgood carbon black dispersion is obtained.6.2 Test Method AInternal Mixer for Initial and FinalMixSee Table 2 and Table 3.6.2.1 For general mixing
16、procedure, refer to PracticeD3182.6.2.1.1 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 D5289.6.2.1.2 If tensile stress strain
17、 tests are required, sheet off toa finished thickness of approximately 2.2 mm (0.087 in.) andcondition the compound according to Practice D3182.6.3 Test Method BInternal Mixer for Initial Mix WithFinal Mill Mix:6.3.1 For general mixing procedure refer to Practice D3182.6.3.2 Mixing CycleInitial Mix:
18、6.3.2.1 Prepare the initial mix in accordance with theprocedure outlined in Table 2.6.3.3 Final MixSee Table 4.6.3.3.1 After mixing according to Table 4, measure andrecord the batch mass. If it differs from the theoretical value bymore than 0.5 %, discard the batch.6.3.3.2 If required, cut samples f
19、rom 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 D5289.6.3.3.3 If tensile stress strain tests are required, sheet off toa finished thickness of approximate
20、ly 2.2 mm (0.087 in.) andcondition the compound according to Practice D3182.6.4 Test Method CMill Procedure:6.4.1 For general mixing procedure, refer to PracticeD3182.6.4.1.1 Pre-blend the zinc oxide and stearic acid in a singlecontainer.6.4.1.2 To simplify the addition of the oil, prepare anoil-car
21、bon black paste as follows: Add the oil to a 100 mLbeaker. While stirring the oil with a spatula, slowly add 30 g ofthe carbon black until a paste is formed.6.4.1.3 Adjust the mill cooling conditions to maintain atemperature of 35 6 5C throughout the mixing operations.TABLE 1 Standard FormulasIRM- Q
22、uantity,SRM Parts byMaterial No. MassBR . 100.00Zinc oxideA3.00SulfurA1.50Stearic acidA2.00Current IRBA60.00TBBSBA0.90ASTM Type 103 petroleum oilCA15.00Total 182.40Batch Factor for mill mixD4.0Batch Factor for internal mixerD7.13Batch Factor for MIM Mix (Cam Head)D,E0.40Batch Factor for MIM Mix (Ban
23、buryHead)D,E0.34AUse the latest IRM/SRM.BN-tert-butyl-2-benzothiazolesulfenamide.CViscosity is 16.8 6 1.2 mm2/s at 100C in accordance with Test Methods D88and Practice D2161. Viscosity Gravity Constant is 0.889 6 0.002 in accordancewith Test Method D2501. Available in 1 and 5-gal (3.8 and 19-L) quan
24、tities fromSun Oil, Industrial Products Dept., 1608 Walnut St., Philadelphia, PA 19103.DFor mill and internal mixer batches, weigh the rubber, carbon black and oil tothe nearest 1.0 g, the sulfur and accelerators to the nearest 0.02 g, and the othercompounding materials to the nearest 0.1 g. For MIM
25、 batches, weigh the rubberand material, blend to the nearest 0.01 g and the individual compoundingmaterials, if used, to the nearest 0.001 g.EFor the MIM procedure, it is recommended that a blend of compoundingmaterials, excluding carbon black and oil, be prepared to improve accuracy in theweighing
26、of these materials. The material blend is prepared by blending aproportional mass of each material in a dry powder blender such as a biconicalblender or vee blender. A mortar and pestle may be used for blending smallquantities.TABLE 2 Internal Mixer Method AInitial MixDuration, min Accumulative, min
27、Adjust the internal mixer temperature to achieve the dischargeconditions outlined below. Close the discharge gate, start the rotor,at 8.0 rads/s (77 r/min) and raise the ram.0.0 0.0Charge one half the rubber, all of the zinc oxide, carbon black, oil,stearic acid, and then the other one half of the r
28、ubber. Lower theram.0.5 0.5Allow the batch to mix. 3.0 3.5Raise the ram and clean the mixer throat and the top of the ram.Lower the ram.0.5 4.0Allow the batch to mix until a temperature of 170C (338F) or atotal mixing time of 6 min is reached, whichever occurs first.Discharge the batch. Subtotal tim
29、e (min) max.2.0 6.0Check the batch mass and record. If it differs from the theoreticalvalue by more than 0.5 %, discard the batch.0.0 0.0Pass the batch immediately through the standard laboratory millthree times, set at 6.0 mm (0.25 in.) and 40 6 5C (104 6 9F).1.0 7.0Allow the stock to rest for 1 to
30、 24 h. 0.0 0.0D3189 06 (2011)2Adjust the mill openings as necessary to maintain a goodrolling bank at the nip of the rolls during the mixing.6.4.2 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
31、 0.5 %, discard the batch.6.4.2.2 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 Methods D2084 or D5289.6.4.2.3 If tensile stress strain tests a
32、re required, sheet off toa finished thickness of approximately 2.2 mm (0.087 in.) andcondition the compound according to Practice D3182.6.5 Test Method DMiniature Internal Mixer (MIM) Pro-cedure:6.5.1 For general mixing procedure, refer to PracticeD3182.6.5.2 Mix with the head temperature of the min
33、iatureinternal mixer maintained at 60 6 3C (140 6 5F) and therotor speed set at 6.3 to 6.6 rad/s (60 to 63 r/min).6.5.3 Prepare the rubber by passing it through a mill onetime with the temperature set at 40 6 5C (109 6 9F) and anopening that would give approximately 5 mm (0.2 in.) thicksheet. Cut th
34、e sheet into strips that are approximately 25 mm (1in.) wide. Mix according to the procedure in 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
35、Immediately pass the discharge from the mixertwice 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 openin
36、g of 0.8 mm (0.31 in.) to enhance the dispersion.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 Me
37、thods D1646 or D6204, and vulcanization char-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.TABLE 3 Internal Mix
38、er Method AFinal MixDuration, min Accumulative, minAdjust the internal mixer to 40 6 5C (104 6 9F). Turn off steamand turn on full cooling water to the rotors, start the motor at 8.0rads/s (77 r/min) and raise the ram.0.0 0.0Charge one half the masterbatch, with all the sulfur and acceleratorrolled
39、into this portion of the masterbatch before feeding to themixer. Add the remaining portion of the masterbatch. Lower the ram.0.5 0.5Allow the batch to mix until a temperature of 110 6 5C (230 6 9F)or a total mixing time of 3 min is reached, whichever occurs first.Discharge the batch. Subtotal Time (
40、min) max.2.5 3.0Check the batch mass and record. If it differs from the theoreticalvalue by more than 0.5 %, discard the batch.0.0 0.0Set with the rolls of a standard laboratory mill maintained at 40 65C (104 6 9F) and at 0.8 mm (0.032 in.) opening. Pass the rolledstock endwise through the mill six
41、times.2.0 5.0Open the mill to give a minimum stock thickness of 6 mm (0.25 in.)and pass the stock through the rolls four times, folding it back onitself each time.1.0 6.0TABLE 4 Test Method BFinal MixDuration, min Accumulative, minWith the roll maintained at 40 6 5C (104 6 9F) and set at 1.5 mm(0.06
42、 in.) opening, band, on the slow roll, the amount of masterbatchbased on two times the formula.0.0 0.0Add slowly the required amount of sulfur and accelerator. 1.0 1.0Make three34 cuts from each side. 2.0 3.0Cut the batch from the mill, and set the mill-roll opening at 0.8 mm(0.032 in.) and pass the
43、 rolled stock endwise through the mill sixtimes.2.0 5.0Open the mill to give a minimum stock thickness of 6 mm (0.25 in.)and pass the stock through the rolls four times, folding it back onitself each time.1.0 6.0D3189 06 (2011)37. Preparation and Testing of Vulcanizates7.1 For stress-strain testing,
44、 prepare the test sheets andvulcanize them in accordance with Practice D3182.7.1.1 The recommended standard vulcanization times forthe mixes prepared by Test MethodsA, B and C are 25, 35, and50 min at 145C (293F). The recommended cure time for theminiature internal mixer compound is 35 min at 145C(2
45、93F).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; however, slightly differentresults may be obtained.7.1.3 Prepare the test specimens and obtain the mo
46、dulus,tensile, and elongation parameters in accordance with TestMethod D412.7.2 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 C
47、ure 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 temperature, 30-min test time, and nopreheating. The r
48、ecommended Test Method D5289 test condi-tions are 1.67 Hz (100 cpm) oscillation frequency, 0.5oscillation amplitude, 160 C die temperature, 30-min testtime, and no preheating. Test condition tolerances are specifiedby the test methods.7.2.2 The recommended standard test parameters are ML,MH, tsl, t5
49、0, and t90.TABLE 5 Test Method CMixing CycleNOTEDo not cut the batch while any free ingredient is evident in the bank or on the milling surface.Duration, min Accumulative, minWith rolls temperature set at 35 6 5C and opening of 0.46 mmband the rubber on the front roll.1.5 1.5Add the preblended zinc oxide and stearic acid evenly across therolls. Make two34 cuts from each side.2.5 4.0Add a small amount of dry carbon black evenly across the rolls,then using a spatula, wipe some of the oil-carbon black paste on tothe mix
