1、Designation: D 3192 05Standard Test Methods forCarbon Black Evaluation in NR (Natural Rubber)1This standard is issued under the fixed designation D 3192; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A
2、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, testformulation, mixing procedure, and test methods for theevaluation and production
3、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 theresponsibility of
4、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:2D 412 Test Methods for Vulcanized Rubber and Thermo-plastic ElastomersTensionD 1799 Practice for Carbon B
5、lackSampling PackagedShipmentsD 1900 Practice for Carbon BlackSampling Bulk 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 She
6、etsD 4483 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 rubber pro
7、ducts. 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 for the
8、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. Standard Te
9、st 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 CMiniature Int
10、ernal 0.40Mixer_AIRM 91 is available from R. E. Carroll, Inc., 1570 North OldenAve.,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 satisfactory perf
11、ormance. 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 in the N-800
12、 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 PracticeD 1799 or Practice D 1900.5.2 The carbon
13、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 onCarbon Black a
14、nd are the direct responsibility of Subcommittee D24.71 on CarbonBlack Testing in Rubber.Current edition approved June 1, 2005. Published June 2005. Originallyapproved in 1973. Last previous edition approved in 2002 as D 3192 - 02.2For referenced ASTM standards, visit the ASTM website, www.astm.org,
15、 orcontact ASTM Customer Service at serviceastm.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.conditioning. T
16、he 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 D 3182.The following mixing procedures are acceptable in testingcarbon black: (1) Test Method AMill Mix, (2) Test MethodBInt
17、ernal Mixer, and (3) Test Method CMiniature InternalMixer.6.2 Mill MixTest Method A: Duration, min Accumulative,min6.2.1 Set the mill opening at 1.4 mm (0.055 in.) and adjust and maintain roll temperature at 70 6 5C. 0 06.2.2 Add rubber and band on the front roll. Make two34 cuts from each side. 2.0
18、 2.06.2.3 Set mill opening at 1.65 mm (0.065 in.). Add stearic acid. Make one34 cut from each side. 2.5 4.56.2.4 Add sulfur, accelerator, and zinc oxide. Make two34 cuts from each side. 2.0 6.56.2.5 Add all the black. When that portion of the carbon black that was added has dropped through to the mi
19、ll pan and thebank is dry, make two34 cuts from each side. Open the mill to 1.9 mm (0.075 in.) and add the carbon black from the mill panuntil all is incorporated. Make three34 cuts from each side. 7.5 14.0NoteDo not cut any stock while free carbon black is evident in the bank or on the milling surf
20、ace. Be certain to return anypigments that drop through the mill to the milling stock.6.2.6 Set the mill opening at 0.80 mm (0.032 in.) and pass the rolled batch endwise through the mill six times. 2.0 16.06.2.7 Open the mill to give a minimum stock thickness of 6 mm (0.25 in.) and pass the stock th
21、rough the rolls four times,folding it back on itself each time. 1.0 17.0Total Time 17.06.2.8 Check the batch mass and record. If outside of the range from 641.2 to 647.6 g, reject the batch. From this stock, cutenough sample to allow testing of or curing characteristics in accordance with Test Metho
22、d D 2084, if desired.6.2.9 Open the mill and sheet off to produce a thickness of 2.2 mm (0.085 in.).6.2.10 Cool on a flat, dry metal surface, at a temperature of 23 6 3C for 1 to 24 h. Unless the relative humidity of thelaboratory is controlled at 50 6 5 %, the sheeted stock should be cooled and sto
23、red in a closed container to prevent moistureabsorption.6.3 Internal MixerTest Method B:6.3.1 Adjust the internal mixer temperature to create in 6.3.8 a dump temperature between 110 and 125C. Close the dis-charge gate, start the rotor, raise the ram, and charge the materials as described. Lower the
24、ram after each operation. 0 06.3.2 Add the rubber. 0.5 0.56.3.3 Add the benzothiazyl disulfide. 0.5 1.06.3.4 Add the stearic acid. 1.0 2.06.3.5 Add the zinc oxide and one-half the carbon black. 1.5 3.56.3.6 Add the remainder of the carbon black. 1.5 5.06.3.7 Add the sulfur. Clean the mixer throat an
25、d the top of the ram. 1.0 6.06.3.8 Dump at 7 min. 1.0 7.0Subtotal 7.06.3.9 Set the mill opening at 0.80 mm (0.032 in.) and maintain the roll temperature at 70 6 5C. Pass the rolled batch end-wise through the mill six times. 2.0 9.06.3.10 Open the mill to give a minimum stock thickness of 6 mm (0.25
26、in.) and pass the stock through the rolls four times,folding it back on itself each time. 1.0 10.0Total Time 10.06.3.11 Check the batch mass and record. If outside of the range from 961.8 to 971.4 g, reject the batch. From this stock,cut enough sample to allow testing of curing characteristics in ac
27、cordance with Test Method D 2084, if desired.6.3.12 Open the mill and sheet off to produce a stock thickness of 2.2 mm (0.085 in.).6.3.13 Cool on a flat, dry metal surface, at a temperature of 23 6 3C for 1 to 24 h. Unless the relative humidity of thelaboratory is controlled at 50 6 5 %, the sheeted
28、 stock should be cooled and stored in a closed container to prevent moistureabsorption.6.4 Miniature Internal MixerTest Method C:6.4.1 Pigment Masterbatch PreparationMill Mix: (Batch Factor 4.00) Set the mill opening at 1.4 mm (0.055 in.) and adjustand maintain roll temperature at 70 6 5C. 0.0 0.06.
29、4.2 Add rubber and band on the front roll. Make two34 cuts from each side. 2.0 2.06.4.3 Set mill opening at 1.65 mm (0.065 in.). Add stearic acid. Make one34 cut from each side. 2.5 4.56.4.4 Add sulfur, accelerator, and zinc oxide. Make two34 cuts from each side. 2.0 6.56.4.5 Set the mill opening at
30、 0.80 mm (0.032 in.), and pass the rolled batch endwise through the mill six times. 2.0 8.56.4.6 Check the batch mass and if outside of the range from 442.2 to 446.6 g, reject the batch. 0.5 9.06.4.7 Set the mill opening to 1.5 mm (0.060 in.), band the stock. Sheet off. 1.0 10.0Total Time 10.06.4.8
31、Cool on a flat, dry metal surface, at a temperature of 23 6 3C. Unless the relative humidity of the laboratory is con-trolled at 50 6 5 %, this masterbatch should be cooled and stored in a closed container to prevent moisture absorption.NoteThis pigment masterbatch should be used within 6 weeks or d
32、iscarded and a new batch prepared.6.4.9 Carbon BlackMiniature Internal Mixer: Mix with the head temperature of the miniature internal mixer maintained at60 6 3C and the unloaded slow rotor speed at 6.3 to 6.6 rad/s (60 to 63 r/min).6.4.10 Cut the pigment masterbatch prepared in 6.4.1 into strips app
33、roximately 20-mm (0.75-in.) wide and weigh out 44.44g.6.4.11 Weigh out 20.00 g of carbon black sample.6.4.12 Charge the mixing chamber with the masterbatch strips, and start the timer. 0.0 0.06.4.13 Masticate the masterbatch. 0.5 0.56.4.14 Add carbon black, use ram to work all of sample into chamber
34、, sweep down orifice and lower ram. 1.0 1.56.4.15 Allow the batch to mix. 1.5 3.0Total Time 3.0D31920526.4.16 Turn off the motor, raise the ram, remove the mixing chamber and unload the batch. Record the batch temperature ifdesired.6.4.17 With the mill at room temperature, pass the batch through the
35、 mill set at 0.80 mm (0.032 in.). Fold it on itself andfeed it back through the mill five more times, always keeping the grain in the same direction and folding it on itself each time.6.4.18 Check the batch mass and record. If outside of the range from 64.12 to 64.76 g, reject the batch.6.4.19 For t
36、esting of stress-strain, pass the batch through the mill to produce a stock thickness of 2.2 mm (0.085 in.).6.4.20 For testing of curing characteristics in accordance with Test Method D 2084, pass the batch through the mill to pro-duce a minimum stock thickness of 6 mm (0.25 in.).6.4.21 Cool on a fl
37、at, dry metal surface, at a temperature of 23 6 3C for 1 to 24 h. Unless the relative humidity of thelaboratory is controlled at 50 6 5 %, the sheeted stock should be cooled and stored in a closed container to prevent moistureabsorption.7. Preparation and Testing of Vulcanizates7.1 For stress-strain
38、 testing, prepare test slabs and vulcanizethem in accordance with Practice D 3182.7.1.1 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 the cured sheets for 1 to 96 h at a tempera-ture of 23 6 3C.7.1
39、.3 Prepare test specimens in accordance with PracticeD 3182 and obtain tensile stress at 300 % elongation, tensilestrength, and ultimate elongation parameters in accordancewith Test Methods D 412. Typically, a test specimen is pre-pared using the current Industry Reference Black, for exampleIRB 7, w
40、ith each set of mixes and the data obtained is reportedas a difference from the IRB.7.2 For measuring vulcanization parameters by the cureme-ter in accordance with Test Method D 2084, use the 6-mm(0.25-in.) thickness samples that were previously prepared.7.2.1 The recommended standard test condition
41、s are 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, t8c(50) and t8c(90).8. Precision and Bias38.1 This precision and bias statement has been prepared ina
42、ccordance with Practice D 4483. Refer to Practice D 4483 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 particu
43、lar interlaboratory 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 Mi
44、ll MixTest 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
45、accordance with Test Method 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 Meth
46、ods D 3192 Method A (using TestMethods D 412 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 population
47、s. Such a decision dictates thatsome appropriate action be taken.8.3.1.2 Tensile StrengthThe pooled repeatability of TestMethods D 3192 MethodA(using Test Methods D 412 MethodA) tensile strength has been established as 1.70 MPa (246 psi).Two single test results (or determinations) that differ by mor
48、ethan 1.70 MPa (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 D 3192 Method A (using Test Methods D 412Method A) ultimate el
49、ongation 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 thatsome appropriate action be taken.8.3.2 Reproducibility:8.3.2.1 Tensile Stress at 300 % ElongationThe pooledreproducibility of Test Methods D 3192 Method A (using TestMethods D 412 Method A) tensile stress at 300 % elongationhas been established as 1.09 MPa (158 psi). Two single testresults (or determin
