1、Designation: D3192 09 (Reapproved 2014)Standard Test Methods forCarbon Black Evaluation in NR (Natural Rubber)1This standard is issued under the fixed designation D3192; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of l
2、ast 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, testformulation, mixing procedure, and test methods for theevaluation
3、and production control of carbon blacks in naturalrubber (NR).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, associated with its use. It is theres
4、ponsibility 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 Thermoplas-tic ElastomersTensionD1799 Practice
5、 for Carbon BlackSampling PackagedShipmentsD1900 Practice for Carbon BlackSampling Bulk Ship-mentsD2084 Test Method for Rubber PropertyVulcanizationUsing Oscillating Disk Cure MeterD3182 Practice for RubberMaterials, Equipment, and Pro-cedures for Mixing Standard Compounds and PreparingStandard Vulc
6、anized SheetsD4483 Practice for Evaluating Precision for Test MethodStandards in the Rubber and Carbon Black ManufacturingIndustries3. Significance and Use3.1 The major portion of carbon black consumed by therubber industry is used to improve the physical properties, lifeexpectancy, and utility of r
7、ubber products. These test methodsprovide a natural rubber formulation and directions for evalu-ating carbon black intended for use in rubber products.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
8、 for the quality assurance ofcarbon black production. They may also be used 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.4. St
9、andard Test Formula4.1 Standard Formula:Material IRMANo. Quantity, partsby massNatural rubberB. 100.00Stearic acid 21 3.00Zinc oxide 91 5.00Benzothiazyl disulfide 2 0.60Sulfur 31 2.50Carbon blackC. 50.00Total 161.10Batch factor:DTest Method AMill 4.00Test Method BInternal Mixer 6.00Test Method CMini
10、ature Internal 0.40Mixer_AIRM 91 is available from R. E. Carroll, Inc., 1570 North Olden Ave., Trenton, NJ08638; (800) 2579365. IRM 2, IRM 21, and IRM 31 are available from AkronRubber Development Lab, 2887 Gilchrist Road, Akron, OH 44305; (330)7946600.BSMR L and STR L have been found to give satisf
11、actory performance. Othersources of rubber may give satisfactory results but have not been investigated bySubcommittee D24.71. Other sources of rubber should be checked to ensure thatresults equivalent to SMR L are attained before using in this test method.CUse 75.00 parts by mass of carbon blacks i
12、n the N-800 and N-900 series.DWeigh rubber and carbon black to the nearest 1 g, sulfur and accelerator to thenearest 0.02 g, and all other compounding materials to the nearest 0.1 g.5. Sampling and Sample Preparation5.1 Samples shall be taken in accordance with PracticeD1799 or Practice D1900.5.2 Th
13、e carbon black shall be conditioned before weighingand mixing by heating for1hinanoven set at 125 6 1C. Theblack shall be placed in an open vessel of suitable dimensionsso that the depth of black is no more than 10 mm during1These test methods are under the jurisdiction of ASTM Committee D24 onCarbo
14、n Black and are the direct responsibility of Subcommittee D24.71 on CarbonBlack Testing in Rubber.Current edition approved Sept. 1, 2014. Published November 2014. Originallyapproved in 1973. Last previous edition approved in 2009 as D3192 09. DOI:10.1520/D3192-09R14.2For referenced ASTM standards, v
15、isit 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.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-
16、2959. United States1conditioning. The black conditioned as above shall be stored ina closed moisture-proof container until ready for mixing.6. Mixing Procedures6.1 For general mixing procedure refer to Practice D3182.The following mixing procedures are acceptable in testingcarbon black: (1) Test Met
17、hod AMill Mix, (2) Test MethodBInternal Mixer, and (3) Test Method CMiniature InternalMixer.6.1.1 Test Method AMill Mix:Duration,minAccumulative,minSet the mill opening at 1.4 mm (0.055 in.) andadjust and maintain roll temperature at 70 5C. 0 0Add rubber and band on the front roll.Make two34 cuts fr
18、om each side. 2.0 2.0Set mill opening at 1.65 mm (0.065 in.).Add stearic acid.Make one34 cut from each side. 2.5 4.5Add sulfur, accelerator, and zinc oxide.Make two34 cuts from each side. 2.0 6.5Add all the black.When that portion of the carbon black that wasadded has dropped through to the mill pan
19、 and thebank is dry, make two34 cuts from each side.Open the mill to 1.9 mm (0.075 in.) and add thecarbon black from the mill pan until all isincorporated.Make three34 cuts from each side. 7.5 14.0NoteDo not cut any stock while free carbon blackis evident in the bank or on the milling surface. Becer
20、tain to return any pigments that drop through themill to the milling stock.Set the mill opening at 0.80 mm (0.032 in.) andpass the rolled batch endwise through the mill sixtimes. 2.0 16.0Open the mill to give a minimum stock thickness of6 mm (0.25 in.) and pass the stock through the rollsfour times,
21、 folding it back on itself each time. 1.0 17.0Total Time 17.06.1.1.1 Check the batch mass and record. If outside of therange from 641.2 to 647.6 g, reject the batch. From this stock,cut enough sample to allow testing of or curing characteristicsin accordance with Test Method D2084, if desired.6.1.1.
22、2 Open the mill and sheet off to produce a thickness of2.2 mm (0.085 in.).6.1.1.3 Cool on a flat, dry metal surface, at a temperature of23 6 3C for 1 to 24 h. Unless the relative humidity of thelaboratory is controlled at 50 6 5 %, the sheeted stock shouldbe cooled and stored in a closed container t
23、o prevent moistureabsorption.6.1.2 Test Method BInternal Mixer:Duration,minAccumulative,minAdjust the internal mixer temperature to create adump temperature between 110 and 125C.Close the discharge gate, start the rotor, raise theram, and charge the materials as described.Lower the ram after each op
24、eration. 0 0Add the rubber. 0.5 0.5Add the benzothiazyl disulfide. 0.5 1.0Add the stearic acid. 1.0 2.0Add the zinc oxide and one-half the carbon black. 1.5 3.5Add the remainder of the carbon black. 1.5 5.0Add the sulfur. Clean the mixer throat and the top ofthe ram. 1.0 6.0Dump at 7 min. 1.0 7.0Sub
25、total 7.0Set the mill opening at 0.80 mm (0.032 in.) andmaintain the roll temperature at 70 5C.Pass the rolled batch endwise through the mill sixtimes. 2.0 9.0Open the mill to give a minimum stock thickness of6 mm (0.25 in.) and pass the stock through the rollsfour times, folding it back on itself e
26、ach time. 1.0 10.0Total Time 10.06.1.2.1 Check the batch mass and record. If outside of therange from 961.8 to 971.4 g, reject the batch. From this stock,cut enough sample to allow testing of curing characteristics inaccordance with Test Method D2084, if desired.6.1.2.2 Open the mill and sheet off t
27、o produce a stockthickness of 2.2 mm (0.085 in.).6.1.2.3 Unless otherwise specified, condition 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
28、from the air, or in an area controlled at35 6 5 % relative humidity in accordance with PracticeD3182. Vulcanize and test in accordance with Section 7.6.1.3 Test Method CMiniature Internal Mixer:6.1.3.1 Pigment Masterbatch PreparationMill Mix:Duration,minAccumulative,min(Batch Factor 4.00) Set the mi
29、ll opening at 1.4 mm(0.055 in.) and adjust and maintain roll temperatureat 70 5C. 0.0 0.0Add rubber and band on the front roll.Make two34 cuts from each side. 2.0 2.0Set mill opening at 1.65 mm (0.065 in.).Add stearic acid.Make one34 cut from each side. 2.5 4.5Add sulfur, accelerator, and zinc oxide
30、.Make two34 cuts from each side. 2.0 6.5Set the mill opening at 0.80 mm (0.032 in.), andpass the rolled batch endwise through the mill sixtimes. 2.0 8.5Check the batch mass and if outside of the rangefrom 442.2 to 446.6 g, reject the batch. 0.5 9.0Set the mill opening to 1.5 mm (0.060 in.), band the
31、stock. Sheet off. 1.0 10.0Total Time 10.0(1) Cool on a flat, dry metal surface, at a temperature of 236 3C. Unless the relative humidity of the laboratory iscontrolled at 50 6 5 %, this masterbatch should be cooled andstored in a closed container to prevent moisture absorption.NOTE 1This pigment mas
32、terbatch should be used within 6 weeks ordiscarded and a new batch prepared.6.1.3.2 Carbon BlackMiniature Internal Mixer:D3192 09 (2014)2(1) Mix with the head temperature of the miniature internalmixer maintained at 60 6 3C and the unloaded slow rotorspeed at 6.3 to 6.6 rad/s (60 to 63 r/min).(2) Cu
33、t the pigment masterbatch prepared in 6.4.1 intostrips approximately 20-mm (0.75-in.) wide and weigh out44.44 g.(3) Weigh out 20.00 g of carbon black sample.Duration,minAccumulative,minCharge the mixing chamber with the masterbatchstrips, and start the timer. 0.0 0.0Masticate the masterbatch. 0.5 0.
34、5Add carbon black, use ram to work all of sampleinto chamber, sweep down orifice, and lower ram. 1.0 1.5Allow the batch to mix. 1.5 3.0Total Time 3.0(4) Turn off the motor, raise the ram, remove the mixingchamber and unload the batch. Record the batch temperature ifdesired.(5) With the mill at room
35、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 on itself eachtime.(6) Check the batch mass and record. If outside of the rangefrom 64.12 to 64.76
36、g, reject the batch.(7) For testing of stress-strain, pass the batch through themill to produce a stock thickness of 2.2 mm (0.085 in.).(8) For testing of curing characteristics in accordance withTest Method D2084, pass the batch through the mill to producea minimum stock thickness of 6 mm (0.25 in.
37、).(9) Cool on a flat, dry metal surface, at a temperature of 236 3C for 1 to 24 h. Unless the relative humidity of thelaboratory is controlled at 50 6 5 %, the sheeted stock shouldbe cooled and stored in a closed container to prevent moistureabsorption.7. Preparation and Testing of Vulcanizates7.1 F
38、or stress-strain testing, prepare test slabs and vulcanizethem in accordance with Practice D3182.7.1.1 The recommended standard cures are 30 min at 145Cfor ASTM N-type carbon black, and 30 and 50 min at 145Cfor ASTM S-type carbon black.7.1.2 Condition vulcanizates of compounds at a temperatureof 23
39、6 2C (73 6 3.6F) for at least 16 h and for not morethan 96 h before preparing and testing, unless otherwisespecified.NOTE 2Quality control of rubber production may require testingwithin 1 to6htoprovide close surveillance of the plant operation;however, slightly different results may be obtained.7.1.
40、3 Prepare test specimens in accordance with PracticeD3182 and obtain tensile stress at 300 % elongation, tensilestrength, and ultimate elongation parameters in accordancewith Test Methods D412. Typically, a test specimen is preparedusing the current Industry Reference Black, for example IRB 7,with e
41、ach set of mixes and the data obtained is reported as adifference from the IRB.7.2 For measuring vulcanization parameters by the cureme-ter in accordance with Test Method D2084, use the 6-mm(0.25-in.) thickness samples that were previously prepared.7.2.1 The recommended standard test conditions are
42、1.7 Hz(100 cpm) oscillation frequency, 1 6 0.03 amplitude ofoscillation, and 160 6 0.3C die temperature using the microdie system.7.2.2 The recommended standard test parameters are ML,MH, ts1, tc(50) and tc(90).8. Precision and Bias38.1 This precision and bias statement has been prepared inaccordanc
43、e with Practice 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, and soforth) used in the particular interl
44、aboratory program describedin 8.3 through 8.5.2.3. The precision parameters should not beused for acceptance or rejection testing of any group ofmaterials without documentation that they are applicable tothose particular materials and the specific testing protocols ofthe test method.8.3 Mill MixTest
45、 Method AA Type 2 interlaboratoryprecision program was conducted in 1990. Both repeatabilityand reproducibility represent short-term testing conditions.Nine 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
46、 with Test Methods D412 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 D3192
47、Method A (using TestMethods D412 Method A) tensile stress at 300 % elongationhas been established as 1.01 MPa (146 psi). Two single testresults (or determinations) that differ by more than 1.01 MPa(146 psi) must be considered suspect, that is, to have comefrom different sample populations. Such a de
48、cision dictates thatsome appropriate action be taken.8.3.1.2 Tensile StrengthThe pooled repeatability of TestMethods D3192 Method A (using Test Methods D412 MethodA) tensile strength has been established as 1.70 MPa (246 psi).Two single test results (or determinations) that differ by morethan 1.70 M
49、Pa (246 psi) must be considered suspect, that is, tohave come from different sample populations. Such a decisiondictates that some appropriate action be taken.8.3.1.3 Ultimate ElongationThe pooled repeatability ofTest Methods D3192 Method A (using Test Methods D412Method A) ultimate elongation has been established as 28.2 %.Two single test results (or determinations) that differ by morethan 28.2 % must be considered suspect, that is, to have comefrom different sample populations. Such a decision dictates thatsom
