1、Designation: D 3191 06e1Standard Test Methods forCarbon Black in SBR (Styrene-Butadiene Rubber)Recipeand Evaluation Procedures1This standard is issued under the fixed designation D 3191; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revisi
2、on, 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.e1NOTEParagraphs 6.2.2.1 and 6.2.2.3 revised editorially in July 2008.1. Scope1.1 These test methods cover the sta
3、ndard materials, testformula, mixing procedure, and test 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 n
4、ot 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 ASTM Standar
5、ds: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 1799 Practice for Carbon BlackSampling PackagedShipmentsD 1900 Practice for Carbon BlackSampling B
6、ulk Ship-mentsD 2084 Test Method for Rubber PropertyVulcanizationUsing Oscillating Disk Cure MeterD 3182 Practice for RubberMaterials, Equipment, andProcedures for Mixing Standard Compounds and Prepar-ing Standard Vulcanized SheetsD 3674 Test Method for Carbon Black Relative ExtrucionMass3D 4483 Pra
7、ctice for Evaluating Precision for Test MethodStandards in the Rubber and Carbon Black ManufacturingIndustriesD 5289 Test Method for Rubber PropertyVulcanizationUsing Rotorless Cure MetersE 145 Specification for Gravity-Convection and Forced-Ventilation Ovens3. Significance and Use3.1 The major port
8、ion of carbon black consumed by therubber industry is 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 avail
9、able elsewhere in the ASTM standards forthe evaluation 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 us
10、ed for thepreparation of reference compounds, to confirm 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
11、Black and are the direct responsibility of Subcommittee D24.71 on CarbonBlack Testing in Rubber.Current edition approved July 1, 2006. Published July 2006. Originally approvedin 1973. Last previous edition approved in 2002 as D 3191 02.2For referenced ASTM standards, visit the ASTM website, www.astm
12、.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.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States
13、.4. 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 R. E. Carroll, Inc., 1570 North Olden Ave., Trenton, NJ086
14、38; (800) 2579365. IRM 21 and IRM 31 are available from Akron RubberDevelopment Lab, 2887 Gilchrist Road, Akron, OH 44305; (330) 7946600.BFor the MIM procedure, it is recommended that a blend of compoundingmaterials be prepared to improve accuracy of the weighing of these materials. Thismaterial ble
15、nd is prepared by blending a proportional mass of each material in adry powder blender such as a biconical blender or vee blender. A mortar and pestlemay be used for blending small quantities.CFor mill mixes, weigh the rubber and carbon black to the nearest 1.0 g, thesulfur and the accelerator to th
16、e 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-benzothiazolesulfenamide.EFor the mill mixes, a batch factor shou
17、ld be selected to the nearest 0.5 to giveas large a total mass as possible that will not exceed 525.0 g. Calculate all partsto the nearest 0.01 part. For MIM mixes, calculate a batch factor to the nearest0.01 that will provide a 75 % loading of the mixing chamber.5. Sampling and Sample Preparation5.
18、1 Samples shall be taken in accordance with PracticeD 1799 or Practice D 1900.5.2 The carbon black shall be conditioned before weighingand mixing by heating in a Type 1B oven, as described inSpecification E 145,for1hat1256 3C. The black shall beplaced in an open vessel of suitable dimensions so that
19、 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 D 3182.6.1.1 Mixing shall be done with the mill roll temperatu
20、remaintained 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, and(3) Test Method CMiniature Internal Mixer.
21、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 D 1646, and curingcharacteristics in accordance with Test Method D 2084,orbot
22、h, and extrudability of unvulcanized compounds in accor-dance with Test Method D 3674, if these are desired.6.2 Mixing Cycle:6.2.1 Test Method AMill Mix:Duration,minAccumula-tive, minSet the mill opening at 1.1 mm (0.045 in.)and band the polymer on the front roll.Make34 cuts every12 min from alterna
23、tesides.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 one half theblack is incorporated, open the
24、 mill to 1.4mm (0.055 in.) and make one34 cut fromeach side. Add the remainder of the car-bon black. When all the black has beenincorporated, open the mill to 1.8 mm(0.070 in.) and make one34 cut fromeach side.10.0 16.0NoteDo not cut any stock while freecarbon black is evident in the bank or onthe m
25、illing 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 (0.032 in.). Passthe rolled stock endwi
26、se 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 setting to givea finished gauge of approxima
27、tely 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 accordance with Practice D 3182.6.2.2 Test Me
28、thod 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 conditions outlinedin the table below
29、. Close the gate.Duration,minAccumula-tive, minRaise ram, add SBR-1500 and zinc ox-ide, and lower ram.0.75 0.75Raise ram, add all other ingredients ex-cept TBBS, and lower ram.D319106e12Raise ram, sweep, lower ram. 1.25 2.0Dump at 3.5 min but not over 71C. 1.5 3.5Total Time 3.56.2.2.3 Mill in accord
30、ance with Practice D 3182, 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 % different from theoretical mass.Durati
31、on,minAccumula-tive, 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 650 g, roll, and pass endwise nine
32、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 To prevent absorption of moisture, condition thesheeted stock for 1 t
33、o8hatatemperature of 23 6 3C in aclosed container after cooling unless the relative humidity iscontrolled at 35 6 5 % in accordance with Practice D 3182.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
34、 onetime with the mill temperature at 50 6 5C and a mill openingat 0.51 mm (0.020 in.).Duration,minAccumula-tive, minWith the head temperature of the minia-ture internal mixer maintained at 60 6 3Cand the unloaded slow rotor speed at 6.3to 6.6 rad/s (60 to 63 r/min), feed the rub-ber into the mixing
35、 chamber and start thetimer as soon as all the rubber is added.Break down the rubber. While the rubberis breaking down, set the powder chute inplace.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 r
36、am.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 chute 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 mixingch
37、amber, 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 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 o
38、n 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 of 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 acc
39、ordancewith Test Method D 2084, pass the batch through the mill toproduce a minimum stock thickness of 6 mm (0.25 in.).6.2.3.7 To prevent absorption of moisture, condition thesheeted stock for 1 to8hatatemperature of 23 6 3C in aclosed container after cooling unless the relative humidity iscontrolle
40、d at 35 6 5 % in accordance with Practice D 3182.Vulcanize and test in accordance with Section 7.7. Preparation and Testing of Vulcanizates7.1 For stress-strain testing, prepare test slabs and vulcanizethem in accordance with Practice D 3182.7.1.1 The recommended standard cure is 50 min at 145C.7.1.
41、2 Condition the cured sheets for 1 to 96 h at a tempera-ture of 23 6 3C.7.1.3 Prepare the test specimens in accordance with PracticeD 3182, and obtain modulus, tensile, and elongation param-eters in accordance with Test Methods D 412. Typically, a testspecimen is prepared using the current Industry
42、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 properties ofvulcanizates is the cure-meter measurement of vulcanizationparameters with an Oscillating Disk cure meter in accordancewi
43、th Test Method D 2084 or a Rotorless Cure Meter Test inaccordance with Test Method D 5289.7.2.1 The recommended standard Oscillating Disk test con-ditions are: 1.7 Hz oscillation frequency, 61 amplitude ofoscillation, 160C die temperature, 30-min test time, and nopreheating. The recommended test con
44、ditions 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, 30-min test time, and nopreheating. Tolerances for the listed conditions are included inthe specified test methods.7.2.2 The
45、 recommended standard test parameters are ML,MH,ts1,t8c(50), and t8c(90).8. Precision and Bias48.1 This precision and bias statement has been prepared inaccordance with Practice D 4483. Refer to Practice D 4483 forterminology and other statistical details.8.2 PrecisionThe precision results in this p
46、recision andbias section give an estimate of the precision of this testmethod with the materials (rubbers, carbon blacks, etc.) used inthe 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 o
47、f materials4Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR: D24-1030.D319106e13without documentation that they are applicable to those par-ticular materials and the specific testing protocols of the testmethod.8.3 Mill MixTest M
48、ethod 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
49、with Test Methods D 412 and areexpressed as differences from IRB 6. A test result is the valueobtained from a single determination. Acceptable differencevalues were not measured (see Table 1).8.3.1 Repeatability:8.3.1.1 Tensile Stress at 300 % ElongationThe pooledrepeatability of Test Methods D 3191 Method A (using TestMethods D 412 Method A) tensile stress at 300 % elongationhas been established as 0.87 MPa (125 psi). Two single testresults (or determinations) that differ by more than 0.87 MPa(125 psi) must be considered suspect, that
