1、Designation: D3186 07 (Reapproved 2016)Standard Test Methods forRubberEvaluation of SBR (Styrene-Butadiene Rubber)Mixed With Carbon Black or Carbon Black and Oil1This standard is issued under the fixed designation D3186; the number immediately following the designation indicates the year oforiginal
2、adoption or, in the case of revision, 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, testformula, mixing
3、 procedures, and 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 informationonl
4、y.1.3 This standard 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
5、 Documents2.1 ASTM Standards:2D412 Test Methods for 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 Me
6、terD3182 Practice for RubberMaterials, Equipment, and 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 Manufacturing
7、IndustriesD5289 Test Method for Rubber PropertyVulcanizationUsing Rotorless Cure MetersD6204 Test Method for RubberMeasurement of Unvulca-nized Rheological Properties Using Rotorless Shear Rhe-ometers3. Significance and Use3.1 These test methods are intended mainly for refereepurposes but may be use
8、d for 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 F
9、ormulaSee Table 1.5. Sample Preparation5.1 Obtain and prepare the test samples in accordance withPractice D3896.6. 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 Mi
10、x Procedure:6.2.1 For general mixing procedures, refer to PracticeD3182.6.2.2 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
11、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 D5289.6.2.2.3 If tensile stress strain tests are required, sheet off toa finished thickness of approximately 2
12、.2 mm (0.087 in.) andcondition the compound according to Practice D3182.6.3 Miniature Internal Mixer (MIM) Procedure:1These 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 Jun
13、e 1, 2016. Published July 2016. Originally approvedin 1981. Last previous edition approved in 2011 as D3186 07 (2011). DOI:10.1520/D3186-07R16.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards vo
14、lume information, refer to the standards Document Summary page onthe ASTM website.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States16.3.1 For general mixing procedures refer to PracticeD3182.6.3.2 MIM Mixing CycleSee Table 3.6.3.2.1 Aft
15、er mixing according to Table 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 ro
16、ll 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.6.3.2.3 Measure and record the batch mass. If it differs fromthe th
17、eoretical value by more than 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 D1646 or D6204, and vulcanization char-acteristics in accordance with Test Methods D2084 or D5289.6.3.2.5 If t
18、ensile 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 Internal Mixer Procedure:6.4.1 For general mixing procedure refer to Practice D3182.6.4.2 Mixing Cycle-Initial MixSee Table 4.6.4.2.
19、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.6.4.2.2 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
20、6 5C (104 6 9F).6.4.2.3 Allow 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 allow
21、testing of compound viscosity and processability in accordancewith Test Methods D1646 or D6204, and vulcanization char-acteristics in accordance with Test Methods D2084 or D5289.6.4.3.3 If tensile stress strain tests are required, sheet off toa finished thickness of approximately 2.2 mm (0.087 in.)
22、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 cure times for the millmixes are 25, 35, and 50 min at 145C (293F)
23、. The recom-mended cure time for the miniature 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 s
24、urveillance; however, slightly differentresults may be obtained.TABLE 1 Standard Pigmented SBR Test FormulaMaterial SRM/IRM No.AQuantity, Parts by MassMasterbatch . 100 + XB+ YCZinc oxideD,EA3.00SulfurD,1.75Stearic acidD,1.50TBBSE,FA1.25TotalBatch factorG107.50 + X + YAUse current IRM/SRM.BX = parts
25、 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 accuracy of the weighing of these materials. Thismaterial blend is prepared by blending a proportional mass of each
26、 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 1.0 g, the sulfur and theaccelerator to the nearest 0.02 g, and all of the other compounding materials to theneares
27、t 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-benzothiazolesulfenamide.GFor mill mixes, a batch factor should be selected to the nearest 0.5 to give aslarge a total mass as possible th
28、at 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 chamber.TABLE 2 Mill Mixing CycleDuration,minAccumulative,minSet the mill opening at 1.40 mm (0.056 in.)and band the mast
29、erbatch 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 beenincorporated.24Add zinc oxide and TBBS accelerator. 3 7Make three34 cuts from each side and cutthe batch from mill.2
30、9Set 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 through the mill four times, foldingit back on itself each time.112TABLE 3 Miniature Internal Mixer CycleDuration,min
31、Accumulative,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 blendedzinc oxide, sulfur, stearic acid, and TBBS,taking care to avoid any loss. Sweep theorifice and lower the ram.0.5 1
32、.0Allow the batch to mix. 8.0 9.0D3186 07 (2016)27.1.3 Prepare test specimens and obtain modulus, tensileand elongation in accordance with Test Methods D412.7.2 An alternative to measuring vulcanization characteris-tics by means of tensile stress measurement on vulcanizates isthe measurement of vulc
33、anization 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 (100 cpm) oscillation frequency, 1 osci
34、llationamplitude, 160C die temperature, 30-min test time, and nopreheating. The recommended Test Method D5289 test condi-tions 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 byth
35、e test methods.7.2.2 The 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 D4483. Refer to Practi
36、ce D4483 forterminology 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 paramete
37、rs should notbe used for 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 r
38、eproducibility are short 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 test
39、ed in six laboratories 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 MethodD2084.8.5 The precision of these test methods may be expressed inthe format of the follo
40、wing statements that 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
41、given material in routine 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
42、level) must be considered 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
43、method procedures,that differ by more than the tabulated R (for any given level)must be considered to have come from different or nonidenticalsample populations.8.8 Repeatability and reproducibility expressed as a per-centage of the mean level, (r) and (R), have equivalentapplication statements as a
44、bove 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) testTABLE 4 Int
45、ernal 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 of the zincoxide, stearic acid,
46、 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 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. Discha
47、rge the batch.2.0 6.0TABLE 5 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 ram.0.0 0.0Charge one-half of the batch, wi
48、th 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 reached, whichever occurs first.Discharge the b
49、atch.2.5 3.0With the rolls of a standard laboratory millmaintained at 40 5C (104 9F), and setat 0.8 mm (0.032 in.) opening, pass the rolledbatch 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 6.0D3186 07 (2016)3property 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-mi
