1、Designation: D 3186 07Standard Test Methods forRubberEvaluation of SBR (Styrene-Butadiene Rubber)Mixed With Carbon Black or Carbon Black and Oil1This standard is issued under the fixed designation D 3186; the number immediately following the designation indicates the year oforiginal adoption or, in
2、the case of revision, the year 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, testformula, mixing procedures, an
3、d test methods for the evalua-tion and production control of pigmented types of styrene-butadiene rubbers (SBR). This includes the pigmented SBR oilmasterbatches.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 stan
4、dard does not purport to address all 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 A
5、STM Standards:2D 412 Test Methods for Vulcanized Rubber 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 318
6、2 Practice for RubberMaterials, Equipment, andProcedures 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 ManufacturingIndus
7、triesD 5289 Test Method for Rubber PropertyVulcanizationUsing Rotorless Cure MetersD 6204 Test Method for RubberMeasurement of Unvul-canized Rheological Properties Using Rotorless ShearRheometers3. Significance and Use3.1 These test methods are intended mainly for refereepurposes but may be used for
8、 quality control of masterbatchproduction. They may also be used in research and develop-ment work and for comparison of different rubber samples in astandard formula.3.2 These test methods may also be used to obtain values forcustomer acceptance of rubber.4. Standard Test Formula4.1 Standard Formul
9、aSee Table 1.5. Sample Preparation5.1 Obtain and prepare the test samples in accordance withPractice D 3896.6. Mixing Procedures6.1 The compound may be prepared either on a mill,miniature internal mixer, or laboratory internal mixer, althoughslightly different results may be obtained.6.2 Mill Mix Pr
10、ocedure:6.2.1 For general mixing procedures, refer to PracticeD 3182.6.2.2 Mill Mixing CycleSee Table 2.6.2.2.1 After mixing according to Table 2, measure andrecord the batch mass. If it differs from the theoretical value bymore than 0.5 %, discard the batch.6.2.2.2 If required, cut samples from the
11、 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 5289.1These test methods are under the jurisdiction of ASTM Committee D11 onRubber and are the direct responsib
12、ility of Subcommittee D11.23 on SyntheticRubbers.Current edition approved March 1, 2007. Published April 2007. Originallyapproved in 1981. Last previous edition approved in 2006 as D 3186 06.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serv
13、iceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.6.2.2.3 If tensile stress strain tests are required, sh
14、eet off toa finished thickness of approximately 2.2 mm (0.087 in.) andcondition the compound according to Practice D 3182.6.3 Miniature Internal Mixer (MIM) Procedure:6.3.1 For general mixing procedures refer to PracticeD 3182.6.3.2 MIM Mixing CycleSee Table 3.6.3.2.1 After mixing according to Table
15、 3, turn off themotor, raise the ram, remove the mixing chamber and dis-charge the batch. Record the maximum batch temperatureindicated, if desired.6.3.2.2 Immediately pass the discharge from the mixertwice through a standard mill maintained at 50 6 5C (122 69F) with a roll separation of 0.5 mm (0.0
16、20 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.6.3.2.3 Measure and record the batch mass. If it differs fromthe theoretical value by more than
17、 0.5 %, discard the batch.6.3.2.4 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 accordance with Test Methods D 2084 orD 5289.6.3.2.5 If tensile stress strain tests
18、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 Internal Mixer Procedure:6.4.1 For general mixing procedure refer to PracticeD 3182.6.4.2 Mixing Cycle-Initial MixSee Table 4.6.4.2.1 After mixing according t
19、o Table 4, measure andrecord the batch mass. If it differs from the theoretical value bymore than 0.5 %, discard the batch.6.4.2.2 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 40 6 5C (104 6 9F).6.4.2.3 Al
20、low the batch to rest for 1 to 24 h.6.4.3 Final MixSee Table 5.6.4.3.1 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.6.4.3.2 If required, cut samples from the batch to allowtesting of compound viscos
21、ity and processability in accordancewith Test Methods D 1646 or D 6204, and vulcanizationcharacteristics in accordance with Test Methods D 2084 orD 5289.6.4.3.3 If tensile stress strain tests are required, sheet off toa finished thickness of approximately 2.2 mm (0.087 in.) andcondition the compound
22、 according to Practice D 3182.7. Preparation and Testing of Vulcanizates7.1 For stress-strain testing, prepare the test sheets andvulcanize them in accordance with Practice D 3182.TABLE 1 Standard Pigmented SBR Test FormulaMaterial SRM/IRM No.AQuantity, Parts by MassMasterbatch . 100 + XB+ YCZinc ox
23、ideD,EA3.00SulfurD,1.75Stearic acidD,1.50TBBSE,FA1.25TotalBatch factorG107.50 + X + YAUse current IRM/SRM.BX = parts carbon black per 100 parts base polymer.CY = parts oil per 100 parts base polymer.DFor the MIM procedure, it is recommended that a blend of compoundingmaterials be prepared to improve
24、 accuracy of the weighing of these materials. Thismaterial blend is prepared by blending a proportional mass of each material in adry powder blender such as a biconical blender or vee blender.Amortar and pestlemay be used for blending small quantities.EFor mill mixes, weigh the rubber to the nearest
25、 1.0 g, the sulfur and theaccelerator to the nearest 0.02 g, and all of the other compounding materials to thenearest 0.1 g. For MIM mixes, weigh the rubber and material blend to the nearest0.01 g and individual pigments, if used, to the nearest 0.001 g.FTBBS is N-tert-butyl-2-benzothiazolesulfenami
26、de.GFor mill mixes, a batch factor should be selected to the nearest 0.5 to give aslarge a total mass as possible that will not exceed 525.0 g. Calculate all parts to thenearest 0.01 part. For MIM mixes, calculate a batch factor to the nearest 0.01 thatwill provide a 75 % loading of the mixing chamb
27、er.TABLE 2 Mill Mixing CycleDuration,minAccumulative,minSet the mill opening at 1.40 mm (0.056 in.)and band the masterbatch on the slow rollwithout cutting.00Add sulfur slowly and evenly across the millat a uniform rate.22Add stearic acid. Make one34 cut from eachside after the stearic acid has been
28、incorporated.24Add zinc oxide and TBBS accelerator. 3 7Make three34 cuts from each side and cutthe batch from mill.29Set the rolls at 0.8 mm (0.032 in.). Pass therolled stock endwise through the mill sixtimes.211Open the mill to give a minimum stockthickness of 6 mm (0.25 in.) and pass thecompound t
29、hrough the mill four times, foldingit back on itself each time.112TABLE 3 Miniature Internal Mixer CycleDuration,minAccumulative,minCharge the mixing chamber with themasterbatch strips, lower the ram, and startthe timer.0.0 0.0Masticate the masterbatch. 0.5 0.5Raise the ram, and add previously blend
30、edzinc oxide, sulfur, stearic acid, and TBBS,taking care to avoid any loss. Sweep theorifice and lower the ram.0.5 1.0Allow the batch to mix. 8.0 9.0D31860727.1.1 The recommended standard cure times for the millmixes are 25, 35, and 50 min at 145C (293F). The recom-mended cure time for the miniature
31、 internal mixer and theinternal mixer compounds 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 1Quality control of rubber production may require testingwithin 1 to6htoprovide close surveillance; however, slightly differentresult
32、s may be obtained.7.1.3 Prepare test specimens and obtain modulus, tensileand elongation in accordance with Test Methods D 412.7.2 An alternative to measuring vulcanization characteris-tics by means of tensile stress measurement on vulcanizates isthe measurement of vulcanization characteristics in a
33、ccordancewith Test Method 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
34、die temperature, 30-min 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
35、 recommended standard test parameters are ML,MH,ts1, t50, and t90.NOTE 2It is recommended that MH, if applicable, be taken as thetorque value at 30 min.8. Precision and Bias8.1 This precision and bias section has been prepared inaccordance with Practice D 4483. Refer to Practice D 4483 forterminolog
36、y and other statistical calculation details.8.2 The precision results in this precision and bias sectiongive an estimate of the precision of these test methods with thematerials (rubbers) used in the particular interlaboratory pro-gram as described below. The precision parameters should notbe used f
37、or acceptance/rejection testing of any group ofmaterials without documentation that they are applicable tothose particular materials and the specific testing protocols thatinclude these test methods.8.3 A Type 2 (interlaboratory) precision was evaluated.Both repeatability and reproducibility are sho
38、rt term; a periodof a few days separates replicate test results. A test result is theaverage value, as specified by these test methods, obtained onone determination(s) or measurement(s).8.4 Two different materials (SBR rubbers) were used in theinterlaboratory program; were tested in six laboratories
39、 on twodifferent days, by the internal mixer method. The results of theprecision calculations for repeatability and reproducibility aregiven in Table 6, as conducted according to Test MethodD 2084.8.5 The precision of these test methods may be expressed inthe format of the following statements that
40、use an “appropriatevalue” of r, R,(r), or (R), to be used in decisions about testresults. The appropriate value is that value of r or R associatedwith a mean level in Table 6 closest to the mean level underconsideration at any given time for any given test parameter,and for any given material in rou
41、tine testing operations.8.6 RepeatabilityThe repeatability, r, of these test meth-ods has been established as the appropriate value tabulated inTable 6. Two single test results, obtained under normal testmethod procedures, that differ by more than this tabulated r(for any given level) must be consid
42、ered as derived fromdifferent or nonidentical sample populations.8.7 ReproducibilityThe reproducibility, R, of these testmethods has been established as the appropriate value tabu-lated in Table 6. Two single test results obtained in twodifferent laboratories, under normal test method procedures,tha
43、t differ by more than the tabulated R (for any given level)must be considered to have come from different or nonidenticalsample populations.TABLE 4 Internal Mixer - Initial CycleDuration,minAccumulative,minAdjust the internal mixer temperature toachieve the discharge conditions outlinedbelow. Close
44、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, stearic acid, and then the other one-half of the rubber. Lower the ram.0.5 0.5Allow the batch to mix. 3.0 3.5Raise the ram, and clean the mixer throatand the top
45、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 5 Internal Mixer - Final CycleDuration,minAccumulative,minAdjust the internal mixer temperature to 40 65C (104 6 9F), turn
46、 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 batch before feeding to the mixer. Addthe remaining portion of the batch. Lower th
47、eram.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 millmaintained at 40 6 5C (104 6 9F), and setat 0.8 mm (0.032 in.) opening, pass the rolle
48、dbatch endwise through the rolls 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 6.0D31860738.8 Repeatability and reproducibility expressed as a per-centage of the mean level, (r) and (R), h
49、ave equivalentapplication statements as above for r and R. For the (r) and (R)statements, the difference in the two single test results isexpressed as a percentage of the arithmetic mean of the two testresults.8.9 BiasIn test method terminology, bias is the differencebetween an average test value and the reference (or true) testproperty value. Reference values do not exist for these testmethods, since the value (of the test property) is exclusivelydefined by the test methods. Bias therefore cannot be deter-mined.9. Keywords9.1 carbon black
