1、Designation: D3191 10 (Reapproved 2014)Standard Test Methods forCarbon Black in SBR (Styrene-Butadiene Rubber)Recipeand Evaluation Procedures1This standard is issued under the fixed designation D3191; the number immediately following the designation indicates the year oforiginal adoption or, in the
2、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 procedure, and test
3、 methods for the evaluationand production control of carbon blacks in styrene butadienerubber (SBR).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 all of thesafety concerns, if any,
4、 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 Vulcanized Rubber and Thermopl
5、as-tic ElastomersTensionD1646 Test Methods for RubberViscosity, StressRelaxation, and Pre-Vulcanization Characteristics(Mooney Viscometer)D1799 Practice for Carbon BlackSampling PackagedShipmentsD1900 Practice for Carbon BlackSampling Bulk Ship-mentsD2084 Test Method for Rubber PropertyVulcanization
6、Using Oscillating Disk Cure MeterD3182 Practice for RubberMaterials, Equipment, and Pro-cedures for Mixing Standard Compounds and PreparingStandard Vulcanized SheetsD3674 Test Method for Carbon BlackRelative ExtrusionMass (Withdrawn 1999)3D4483 Practice for Evaluating Precision for Test MethodStanda
7、rds in the Rubber and Carbon Black ManufacturingIndustriesD5289 Test Method for Rubber PropertyVulcanizationUsing Rotorless Cure MetersE145 Specification for Gravity-Convection and Forced-Ventilation Ovens3. Significance and Use3.1 The major portion of carbon black consumed by therubber industry is
8、used to improve the physical properties, lifeexpectancy, and utility of rubber products. These test methodsprovide an SBR recipe and directions for evaluating all types ofcarbon black intended for use in rubber products. Otherprocedures are available elsewhere in the ASTM standards forthe evaluation
9、 of carbon black itself.3.2 These test methods may be used to characterize carbonblack in terms of specific properties of the standard compound.These test methods are useful for the quality assurance ofcarbon black production. They may also be used for thepreparation of reference compounds, to confi
10、rm the day-to-dayreliability of testing operations used in the rubber industry, forthe evaluation of experimental compounds, and quality controlof production compounds.1These test methods are under the jurisdiction of ASTM Committee D24 onCarbon Black and are the direct responsibility of Subcommitte
11、e D24.71 on CarbonBlack Testing in Rubber.Current edition approved Sept. 1, 2014. Published November 2014. Originallyapproved in 1973. Last previous edition approved in 2010 as D3191 10. DOI:10.1520/D3191-10R14.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Cust
12、omer 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 historical standard is referenced onwww.astm.org.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700,
13、West Conshohocken, PA 19428-2959. United States14. Standard Test Formula4.1 Standard Formula:Material IRMANo.Quantity,parts bymassSBR-1500 . 100.00Zinc oxideB,C91 3.00SulfurB,C31 1.75Stearic acidB,C21 1.00Carbon black . 50.00TBBSC,D. 1.00TotalBatch factor:E156.75AIRM 91 is available from G. H. Chemi
14、cals, Ltd., 1550 Brouillette St., P.O. Box456, St. Hyacinthe Quebec Canada, J2S 7B8. IRM 21 and IRM 31 are availablefrom Akron Rubber Development Lab, 2887 Gilchrist Road, Akron, OH 44305.BFor the MIM procedure, it is recommended that a blend of compounding materialsbe prepared to improve accuracy o
15、f 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 blending small quantities.CFor mill mixes, weigh the rubber and carbon black to the
16、 nearest 1.0 g, the sulfurand the accelerator to the nearest 0.02 g, and all of the other compoundingmaterials to the nearest 0.1 g. For MIM mixes, weigh the rubber and material blendto the nearest 0.01 g and individual pigments, if used, to the nearest 0.001 g.DTBBS is N-tert-butyl-w-benzothiazoles
17、ulfenamide.EFor the 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
18、mixing chamber.5. Sampling and Sample Preparation5.1 Samples shall be taken in accordance with PracticeD1799 or Practice D1900.5.2 The carbon black shall be conditioned before weighingand mixing by heating in a Type 1B oven, as described inSpecification E145,for1hat1256 3C. The black shall beplaced
19、in an open vessel of suitable dimensions so that thedepth of black is no more than 10 mm during conditioning. Theblack conditioned as above shall be stored in a closed moisture-proof container until ready for mixing.6. Mixing Procedure6.1 For general mixing procedure refer to Practice D3182.6.1.1 Mi
20、xing shall be done with the mill roll temperaturemaintained at 50 6 5C. The indicated mill openings areapproximate and should be adjusted to maintain a goodworking bank at the nip of the rolls. The following threemixing procedures are offered:(1) Test Method AMill Mix,(2) Test Method BInternal Mixer
21、, and(3) Test Method CMiniature Internal Mixer.6.1.1.1 Check and record the stock mass. If it differs fromthe theoretical value by more than 0.5 %, reject the batch. Fromthis stock, cut enough sample to allow testing of compoundviscosity in accordance with Test Methods D1646, and curingcharacteristi
22、cs in accordance with Test Method D2084, or both,and extrudability of unvulcanized compounds in accordancewith Test Method D3674, if these are desired.6.2 Mixing Cycle:6.2.1 Test Method AMill Mix:Duration,minAccumulative,minSet the mill opening at 1.1 mm (0.045 in.)and band the polymer on the front
23、roll.Make34 cuts every12 min from alternatesides.2.0 2.0Add the sulfur slowly and evenly acrossthe mill at a uniform rate.2.0 4.0Add the stearic acid. Make one34 cutfrom each side after the stearic acid hasbeen incorporated.2.0 6.0Add the carbon black evenly across themill at a uniform rate. When on
24、e half theblack is incorporated, open the mill to 1.4mm (0.055 in.) and make one34 cut fromeach side. Add the remainder of thecarbon black. When all the black hasbeen incorporated, open the mill to 1.8mm (0.070 in.) and make one34 cut fromeach side.10.0 16.0NoteDo not cut any stock while freecarbon
25、black is evident in the bank or onthe milling surface. Be certain to returnany pigments that drop through the mill tothe milling stock.Add the zinc oxide and TBBS at the1.8-mm (0.070-in.) setting.3.0 19.0Make three34 cuts from each side andcut the stock from the mill.2.0 21.0Set the rolls at 0.8 mm
26、(0.032 in.). Passthe rolled stock endwise through the millsix times.2.0 23.0Open the mill to give a minimum stockthickness of 6 mm (0.25 in.) and pass thestock through the rolls four times, foldingit back on itself each time.1.0 24.0Total Time 24.06.2.1.1 Sheet off the stock from the mill at a setti
27、ng to givea finished gauge of approximately 2.2 mm (0.085 in.). Cool ona flat dry metal surface.6.2.1.2 To prevent absorption of moisture, condition thesheeted stock for 1 to8hatatemperature of 23 6 3C in aclosed container after cooling unless the relative humidity iscontrolled at 35 6 5 % in accord
28、ance with Practice D3182.6.2.2 Test Method BInternal Mixer:6.2.2.1 BR Banbury: Water cooled (not over 16C) rotors at8.06 rad/s (77 r/min). Start loading when Banbury temperaturerecorder indicates 32C.6.2.2.2 Before mixing the first batch, adjust the internalmixer temperature to achieve the discharge
29、 conditions outlinedin the table below. Close the gate.Duration,minAccumulative,minRaise ram, add SBR-1500 and zincoxide, and lower ram.0.75 0.75Raise ram, add all other ingredientsexcept TBBS, and lower ram.Raise ram, sweep, lower ram. 1.25 2.0Dump at 3.5 min but not over 71C. 1.5 3.5Total Time 3.5
30、D3191 10 (2014)26.2.2.3 Mill in accordance with Practice D3182, 6-by-12 in.mill with water cooling. (Before using the mill warm up witha batch of rubber. Start mill operations when roll surfacetemperature is 32C.)6.2.2.4 Sheet out on the mill, weigh, and check batch mass.Discard if more than 0.5 % d
31、ifferent from theoretical mass.Duration,minAccumulative,minReturn to mill, set at 1.8 mm (0.070 in.)between rolls, band on mill, add TBBS, andmake five34 cuts from each side.2.5 2.5Total Time 2.56.2.2.5 Remove stock from the mill in a sheet and allow torest1honaflat, dry metal surface.6.2.2.6 Weigh
32、650 g, roll, and pass endwise nine times,without banding through the mill set at 0.5 mm (0.020 in.)between rolls. Start with a surface temperature of 32C.6.2.2.7 Sheet out stock to a thickness of about 2.2 mm(0.085 in.) and cool on a flat, dry metal surface.6.2.2.8 Unless otherwise specified, condit
33、ion the sheetedcompound for 1 to 24 h at 23 6 3C (73.4 6 5.4F) at a relativehumidity not greater than 55 %. For maximum precision,condition for 1 to 24 h in a closed container to preventabsorption of moisture from the air, or in an area controlled at35 6 5 % relative humidity in accordance with Prac
34、ticeD3182. Vulcanize and test in accordance with Section 7.6.2.3 Test Method CMiniature Internal Mixer:6.2.3.1 Prepare the rubber by passing it through a mill onetime with the mill temperature at 50 6 5C and a mill openingat 0.51 mm (0.020 in.).Duration,minAccumulative,minWith the head temperature o
35、f theminiature internal mixer maintained at 60 3C and the unloaded slow rotor speedat 6.3 to 6.6 rad/s (60 to 63 r/min), feedthe rubber into the mixing chamber andstart the timer as soon as all the rubber isadded. Break down the rubber. While therubber is breaking down, set the powderchute in place.
36、1.0 1.0Add the sulfur, zinc oxide, stearic acid,and TBBS followed by the carbon black.Quickly insert the ram in the chute andplace a 1-kg mass on the ram.1.0 2.0When the ram positon indicates that thecarbon black has been added, remove thechute and sweep the remaining carbonblack from the ram and ch
37、ute cavity intothe mixing chamber.1.0 3.0Allow the compound to mix. 6.0 9.0Total time 9.06.2.3.2 Turn off the motor, raise the ram, remove the mixingchamber, and unload the batch. Record the batch temperature ifdesired.6.2.3.3 With the mill at room temperature, pass the batchthrough the mill set at
38、0.80 mm (0.032 in.). Fold it on itself andfeed it back through the mill five more times, always keepingthe grain in the same direction and folding it on itself eachtime.6.2.3.4 Check the batch mass and record. Reject the batch ifmore than 60.5 % differ from the theoretical mass.6.2.3.5 For testing o
39、f stress-strain, pass the batch throughthe mill to produce a stock thickness of 2.2 mm (0.085 in.).6.2.3.6 For testing of curing characteristics in accordancewith Test Method D2084, pass the batch through the mill toproduce a minimum stock thickness of 6 mm (0.25 in.).6.2.3.7 To prevent absorption o
40、f moisture, condition thesheeted stock for 1 to8hatatemperature of 23 6 3C in aclosed container after cooling unless the relative humidity iscontrolled at 35 6 5 % in accordance with Practice D3182.Vulcanize and test in accordance with Section 7.7. Preparation and Testing of Vulcanizates7.1 For stre
41、ss-strain testing, prepare test slabs and vulcanizethem in accordance with Practice D3182.7.1.1 The recommended standard cure is 50 min at 145C.7.1.2 Condition vulcanizates of compounds at a temperatureof 23 6 2C (73 6 3.6F) for at least 16 h and for not morethan 96 h before preparing and testing, u
42、nless otherwisespecified.NOTE 1Quality control of rubber production may require testingwithin 1 to6htoprovide close surveillance of the plant operation;however, slightly different results may be obtained.7.1.3 Prepare the test specimens in accordance with PracticeD3182, and obtain modulus, tensile,
43、and elongation parametersin accordance with Test Methods D412. Typically, a testspecimen is prepared using the current Industry ReferenceBlack, for example IRB 7, with each set of mixes and the dataobtained is reported as a difference from the IRB.7.2 An alternative to measuring stress-strain proper
44、ties ofvulcanizates is the cure-meter measurement of vulcanizationparameters with an Oscillating Disk cure meter in accordancewith Test Method D2084 or a Rotorless Cure Meter Test inaccordance with Test Method D5289.7.2.1 The recommended standard Oscillating Disk test con-ditions are: 1.7 Hz oscilla
45、tion frequency, 61 amplitude ofoscillation, 160C die temperature, 30-min test time, and nopreheating. The recommended test conditions for the RotorlessCure Meter are: 1.7 Hz oscillation frequency, 60.5 of arc fortorsional shear cure meters, 6 0.05 mm for linear shear curemeters, 160C die temperature
46、, 30-min test time, and nopreheating. Tolerances for the listed conditions are included inthe specified test methods.7.2.2 The recommended standard test parameters are ML,MH,ts1,tc(50), and tc(90).8. Precision and Bias48.1 This precision and bias statement has been prepared inaccordance with Practic
47、e D4483. Refer to Practice D4483 forterminology and other statistical details.8.2 PrecisionThe precision results in this precision andbias section give an estimate of the precision of this testmethod with the materials (rubbers, carbon blacks, etc.) used in4Supporting data have been filed at ASTM In
48、ternational Headquarters and maybe obtained by requesting Research Report RR:D24-1030.D3191 10 (2014)3the particular interlaboratory program described in 8.3 through8.4.2.3. The precision parameters should not be used foracceptance or rejection testing of any group of materialswithout documentation
49、that they are applicable to those par-ticular materials and the specific testing protocols of the testmethod.8.3 Mill MixTest Method AA Type 2 interlaboratoryprecision program was conducted in 1990. Both repeatabilityand reproducibility represent short-term testing conditions.Seven laboratories tested four carbon blacks (SRBs A-4, B-4,D-4, and F-4) once on each of two different days. Test resultswere obtained in accordance with Test Methods D412 and areexpressed as differences from IRB 6. A test result is the valueobtained from a s
