1、Designation: D3189 06 (Reapproved 2016)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 Thermoplas-tic Elasto
5、mersTensionD1646 Test Methods for RubberViscosity, StressRelaxation, and Pre-Vulcanization Characteristics(Mooney Viscometer)D2084 Test Method for Rubber PropertyVulcanizationUsing Oscillating Disk Cure MeterD2161 Practice for Conversion of Kinematic Viscosity toSaybolt Universal Viscosity or to Say
6、bolt 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 Testing (Withdrawn1987)3D3182 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-ometersNOTE 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 inte
9、nded mainly for 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. Standa
10、rd Test Formula4.1 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
11、 and FinalMix,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 differentresult
12、s may be obtained.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 MethodA, B, or D). The mill procedure (Test Method C) may be used provided1Th
13、ese 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 1973. Last previous edition approved in 2011 as D3189 06 (2011). D
14、OI:10.1520/D3189-06R16.2For 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 ASTM website.3The last approved version of this his
15、torical standard is referenced onwww.astm.org.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1good 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 m
16、ixing 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
17、strain tests are required, sheet off toa finished thickness of approximately 2.2 mm (0.087 in.) andcondition the compound according to Practice D3182.6.3 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 CycleInitia
18、l Mix: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 sam
19、ples 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 D5289.6.3.3.3 If tensile stress strain tests are required, sheet off toa finished thickness of appro
20、ximately 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.TABLE 1 Standard FormulasIRM- Quantity,SRM Parts byMater
21、ial 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 (BanburyHead)D,E0.34AUse the
22、latest IRM/SRM.BN-tert-butyl-2-benzothiazolesulfenamide.CViscosity is 16.8 1.2 mm2/s at 100C in accordance with Test Methods D88 andPractice D2161. Viscosity Gravity Constant is 0.889 0.002 in accordance withTest Method D2501. Available in 1 and 5-gal (3.8 and 19-L) quantities from Sun Oil,Industria
23、l Products Dept., 1608 Walnut St., Philadelphia, PA 19103.DFor mill and internal mixer batches, weigh the rubber, carbon black and oil to thenearest 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 batches, weigh the rubberand
24、 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 of these materials. The mater
25、ial 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, minAdjust the internal mixer tem
26、perature toachieve the discharge conditions outlinedbelow. Close the discharge gate, start therotor, at 8.0 rads/s (77 r/min) and raise theram.0.0 0.0Charge one half the rubber, all of the zincoxide, carbon black, oil, stearic acid, and thenthe other one half of the rubber. Lower theram.0.5 0.5Allow
27、 the batch to mix. 3.0 3.5Raise the ram and clean the mixer throat andthe top of the ram. Lower the ram.0.5 4.0Allow the batch to mix until a temperature of170C (338F) or a total mixing time of 6 minis reached, whichever occurs first. Dischargethe batch. Subtotal time (min) max.2.0 6.0Check the batc
28、h mass and record. If it differsfrom the theoretical value by more than 0.5 %,discard the batch.0.0 0.0Pass the batch immediately through thestandard laboratory mill three times, set at 6.0mm (0.25 in.) and 40 5C (104 9F).1.0 7.0Allow the stock to rest for 1 to 24 h. 0.0 0.0D3189 06 (2016)26.4.1.2 T
29、o simplify the addition of the oil, prepare anoil-carbon 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
30、the mixing operations.Adjust 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 0.5 %,
31、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 are requi
32、red, 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.TABLE 3 Internal Mixer Method AFinal MixDuration, min
33、Accumulative, minAdjust the internal mixer to 40 5C (104 9F). Turn off steam and turn on full coolingwater to the rotors, start the motor at 8.0 rads/s(77 r/min) and raise the ram.0.0 0.0Charge one half the masterbatch, with all thesulfur and accelerator rolled into this portion ofthe masterbatch be
34、fore feeding to the mixer.Add the remaining portion of the masterbatch.Lower the ram.0.5 0.5Allow the batch to mix until a temperature of110 5C (230 9F) or a total mixing time of3 min is reached, whichever occurs first.Discharge the batch. Subtotal Time (min) max.2.5 3.0Check the batch mass and reco
35、rd. If it differsfrom the theoretical value by more than 0.5 %,discard the batch.0.0 0.0Set with the rolls of a standard laboratory millmaintained at 40 5C (104 9F) and at 0.8mm (0.032 in.) opening. Pass the rolled stockendwise through the mill six times.2.0 5.0Open the mill to give a minimum stockt
36、hickness of 6 mm (0.25 in.) and pass the stockthrough 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 5C (104 9F) and set at 1.5 mm (0.06 in.) opening,band, on the slow roll, the amount ofmast
37、erbatch based on two times the formula.0.0 0.0Add slowly the required amount of sulfur andaccelerator.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 passthe rolled stock endwise through the mill sixtimes.2.0 5.0Ope
38、n the mill to give a minimum stockthickness of 6 mm (0.25 in.) and pass thestock through the rolls four times, folding itback on itself each time.1.0 6.0D3189 06 (2016)36.5.2 Mix with the head temperature of the miniatureinternal mixer maintained at 60 6 3C (140 6 5F) and therotor speed set at 6.3 t
39、o 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 the sheet into strips that are approximately 25 mm (1in.) wide. Mix according to the pr
40、ocedure 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 Immediately pass the discharge from the mixertwice through a standard mill maintained
41、 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 (0.31 in.) to enhance the dispersion.6.5.3.3 Measure and record the batch
42、 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-acteristics in accordance with Test Meth
43、ods D2084 or D5289.TABLE 5 Test Method CMixing CycleNOTE 1Do 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 5C and openingof 0.46 mm band the rubber on the front roll.1.5 1.5Add the preblend
44、ed zinc oxide and stearic acidevenly across the rolls. Make two34 cuts from eachside.2.5 4.0Add a small amount of dry carbon black evenlyacross the rolls, then using a spatula, wipe some ofthe oil-carbon black paste on to the mix. Repeat thesequence of dry black addition followed by thepaste until a
45、ll the paste has been added. Use asmall piece of the mix to wipe out the paste con-tainer. Continue to add the dry black slowly untilhalf the black is added. Increase the mill opening to0.6 mm and continue to add the remaining black insmall amounts. Clean the black out of the mill panand add it to t
46、he mix.10.0 14.0Make three34 cuts from each side. 1.5 15.5Add the TBBS and mix until no white spots are vis-ible in the mix. Then slowly add the sulphur evenlyacross the rolls.2.0 17.5Make six successive34 cuts from each side. 2.0 19.5Cut the batch from the mill. Set the mill opening at0.8 mm and pa
47、ss the rolled batch endwise throughthe the rolls six times.2.0 21.5TABLE 6 Test Method DMiniature Internal Mixer ProcedureDuration, min Accumulative, minCharge the mixing chamber with the rubberstrips, lower the ram, and start the timer.0.0 0.0Masticate the rubber. 0.5 0.5Raise the ram, add zinc oxi
48、de, sulfur,stearic acid, and TBBS that have previouslybeen blended, taking care to avoid anyloss.1.0 1.5Add portions of the carbon black and oilalternately, sweep the orifice, and lower theram.1.0 2.5Allow the batch to mix, raising the rammomentarily to sweep down, if necessary.6.5 9.0D3189 06 (2016
49、)46.5.3.5 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, 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 theminiatu
