1、Designation: D 3187 06Standard Test Methods forRubberEvaluation of NBR (Acrylonitrile-ButadieneRubber)1This standard is issued under the fixed designation D 3187; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last rev
2、ision. A 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, testformulas, mixing procedures and test methods for the evalua-tion of vari
3、ous types of acrylonitrile-butadiene rubber (NBR).1.2 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for informationonly.1.3 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibi
4、lity 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:2D 412 Test Methods for Vulcanized Rubber and Thermo-plastic ElastomersTensionD 1646 Test Methods
5、for RubberViscosity, Stress Relax-ation, and Pre-Vulcanization Characteristics (Mooney Vis-cometer)D 2084 Test Method for Rubber PropertyVulcanizationUsing Oscillating Disk Cure MeterD 3182 Practice for RubberMaterials, Equipment, andProcedures for Mixing Standard Compounds and Prepar-ing Standard V
6、ulcanized SheetsD 3896 Practice for Rubber From Synthetic SourcesSamplingD 4483 Practice for Evaluating Precision for Test MethodStandards in the Rubber and Carbon Black ManufacturingIndustriesD 5289 Test Method for Rubber PropertyVulcanizationUsing Rotorless Cure MetersD 6204 Test Method for Rubber
7、Measurement of Unvul-canized Rheological Properties Using Rotorless ShearRheometers3. Significance and Use3.1 These test methods are intended mainly for refereepurposes but may be used for quality control of rubberproduction. They may also be used in research and develop-ment work and for comparison
8、 of different rubber samples in astandard formula.3.2 These test methods may be used to obtain values forcustomer control acceptance of rubber.4. Standard Test Formula4.1 Standard FormulaSee Table 1.5. Sample Preparation5.1 For tests intended for referee purposes obtain andprepare the test samples i
9、n accordance with Practice D 3896.6. Mixing Procedures6.1 The compound may be prepared either on a mill, in aminiature internal mixer, or a lab internal mixer, althoughslightly different results may be obtained.6.2 Mill Procedure:6.2.1 For general mixing procedure refer to PracticeD 3182.6.2.1.1 Mix
10、 with the mill roll temperature maintained at 506 5C (122 6 9F). The indicated mill openings are desiredand should be maintained in so far as possible to provideuniformity in the breakdown of the rubber due to milling.Necessary adjustments may be made to maintain a goodworking bank.6.2.2 Mixing Cycl
11、eSee Table 2.1These 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 March 1, 2006. Published March 2006. Originallyapproved in 1973. Last previous edition approved in 2000 as
12、D 3187 00.2For referenced ASTM standards, visit 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.1Copyright ASTM International, 100 Barr Harbor Driv
13、e, PO Box C700, West Conshohocken, PA 19428-2959, United States.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 the batch to allowtesting of compound visco
14、sity and processability in accordancewith Test Methods D 1646 or D 6204, and vulcanizationcharacteristics in accordance with Test Methods D 2084 orD 5289.6.2.2.3 If tensile stress strain tests are required, sheet off toa finished thickness of approximately 2.2 mm (0.087 in.) andcondition the compoun
15、d according to Practice D 3182.6.3 Miniature Internal Mixer (MIM) Procedure:6.3.1 For general mixing procedure refer to PracticeD 3182.6.3.1.1 Mix with the head temperature of the miniatureinternal mixer maintained at 60 6 3C (140 6 5F) and therotor speed at 6.3 to 6.6 rad/s (60 to 63 r/min).6.3.2 P
16、repare the rubber by passing it through a mill onetime with the temperature set at 50 6 5C (122 6 9F) and anopening that will give an approximately 5 mm (0.2 in.) thicksheet. Cut the sheet into strips that are approximately 25 mm (1in.) wide.6.3.3 Mixing CycleSee Table 3.6.3.3.1 After mixing accordi
17、ng 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.6.3.3.2 Immediately pass the discharge from the mixertwice through a standard mill maintained at 50 6 5C (122 69F) with a roll separation of
18、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 (0.31 in.) to enhance the dispersion.6.3.3.3 Measure and record the batch mass. If it differs fromthe theoretical value b
19、y more than 0.5 %, discard the batch.6.3.3.4 If required, cut samples from the batch to allowtesting of compound viscosity and processability in accordancewith Test Methods D 1646 or D 6204, and vulcanizationcharacteristics in accordance with Test Methods D 2084 orD 5289.6.3.3.5 If tensile stress st
20、rain tests are required, sheet off toa finished thickness of approximately 2.2 mm (0.087 in.) andcondition the compound according to Practice D 3182.6.4 Internal Mixer Procedure:6.4.1 For general mixing procedure refer to PracticeD 3182.6.4.2 Mixing Cycle-Initial MixSee Table 4.6.4.2.1 After mixing
21、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, set at 6.0 mm (0.25 in.) and 40 65C (104 6 9F).6.4.2.3 Allow the batch to rest for
22、 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 allowtesting of compound viscosity and processability in
23、 accordancewith Test Methods D 1646 or D 6204, and vulcanizationcharacteristics in accordance with Test Methods D 2084 orD 5289.6.4.3.3 If tensile stress strain tests are required, sheet off toa finished thickness of approximately 2.2 mm (0.087 in.) andcondition the compound according to Practice D
24、3182.7. Preparation and Testing of Vulcanizates7.1 For stress-strain testing, prepare the test sheets andvulcanize them in accordance with Practice D 3182.7.1.1 The recommended standard cure times for the millcompound are 20, 40, and 60 min at 150C (302F). Therecommended cure time for the miniature
25、internal mixercompound is 40 min at 150C (302F).NOTE 1Vulcanization times of 25, 50, and 75 min at 145C (293F)for the mill compound and 50 min at 145C (293F) for the miniatureinternal mixer compound may also be used, but will not necessarily givethe same results as the recommended standard vulcaniza
26、tion times.7.1.2 Condition the cured sheets for 16 to 96 h at atemperature of 23 6 2C (73.4 6 3.6F).NOTE 2Quality control of rubber production may require testingwithin 1 to6htoprovide close surveillance; however, slightly differentresults may be obtained.7.1.3 Prepare test specimens and obtain modu
27、lus, tensileand elongation parameters in accordance with Test MethodsD 412.7.2 An alternative to measuring vulcanization characteris-tics by means of tensile stress measurement on vulcanizates isthe measurement of vulcanization characteristics in accordancewith Test Methods D 2084 or D 5289. These m
28、ethods will notproduce equal results.TABLE 1 Standard FormulaMaterialNISTSRM/IRM No.Quantity,Parts byMassNBR . 100.00Zinc oxideA3.00Sulfur, coatedB. 1.50Stearic acidA1.00Oil furnace black SRB-B4 40.00TBBSCA0.70Total 146.20Batch factor for mill mixD4.0Batch factor for MIM mix (Cam HeadE0.50Batch fact
29、or for MIM mix (Banbury Head)E0.43AUse current IRM/SRM.BThe use of 2 % MgCO3coated sulfur is recommended. Standard 2 % MgCO3coated sulfur (Lot No. M-266573-P) is available from the C. P. Hall Co., 4460Hudson Drive, Stow, OH 44224.CN-tert-butyl-2-benzothiozolesulfenamide.DFor mill and lab BB mixes, w
30、eigh the rubber and carbon black to the nearest 1.0g, the sulfur and accelerators to the nearest 0.02 g, and all other compoundingmaterials to the nearest 0.1 g.EFor MIM batches, weigh the rubber and material, blend to the nearest 0.1 g. Ifindividual compounding materials are used, blend to the near
31、est 0.001 g. For theMIM procedure, it is recommended that a blend of compounding materials,excluding black, be prepared to improve accuracy in the weighing of thesematerials. The material blend is prepared by blending a proportional mass of eachmaterial in a dry powder blender such as a biconical bl
32、ender or vee blender. Amortar and pestle may be used for blending small quantities.D31870627.2.1 The recommended D 2084 test conditions are 1.67 Hz(100 cpm) oscillation frequency, 1 oscillation amplitude,160C die temperature, 30 min test time, and no preheating.The recommended D 5289 test conditions
33、 are 1.67 Hz oscilla-tion frequency, 0.5 oscillation amplitude, 160C die tempera-ture, 30 min test time, and no preheating. Test conditiontolerances are specified by the test methods.7.2.2 The recommended standard test parameters are ML,MH,tsl,t850, and t890.NOTE 3It is recommended that MH, if appli
34、cable, be taken as thetorque value at 30 min.8. Precision and Bias8.1 This precision and bias section has been prepared inaccordance with Practice D 4483. Refer to Practice D 4483 forterminology and other statistical calculation details.8.2 The precision results in this precision and bias sectiongiv
35、e an estimate of the precision of these test methods with thematerials (rubbers) used in the particular interlaboratory pro-gram as described below. The precision parameters should notbe used for acceptance/rejection testing of any group ofmaterials without documentation that they are applicable tot
36、hose particular materials and the specific testing protocols thatinclude these test methods.8.3 A Type 2 (interlaboratory) precision was evaluated.Both repeatability and reproducibility are short term; a periodof a few days separates replicate test results. A test result forTest Methods D 412 is the
37、 median value, as specified by thesetest methods, obtained on three determination(s) or measure-ment(s). For Test Methods D 1646 and D 2084, a test result isobtained from one determination.8.4 Three different materials or rubbers were used in theinterlaboratory program, these were tested in seven la
38、borato-ries on two different days.8.5 The results of the precision calculations for repeatabilityand reproducibility are given in Table 6.TABLE 2 Mill Procedure: Mixing CycleNOTEDo not cut the batch while free carbon black is evident in the bank or on the milling surface. Be certain to return to the
39、 batch any ingredientsthat drop through the mill.Duration, min Accumulative, minSet the mill opening at 1.4 mm (0.055 in.) and band the rub-ber on the slow roll.22Add stearic acid and zinc oxide together, followed by sulfurand accelerator together. Make the addition slowly andevenly across the mill,
40、 without cutting.35Make three34 cuts from each side. 2 7Add half of the carbon black evenly across the mill at a uni-form rate.512When this portion of the carbon black has been completelyincorporated, open the rolls to 1.65 mm (0.065 in.) andmake three34 cuts from each side.214Add the remaining carb
41、on black evenly across the rolls at auniform rate.519When all carbon black has been incorporated, make three34 cuts from each side221Set the rolls at 0.8 mm (0.032 in.), pass the rolled stockendwise between the rolls six times.324Open the mill to give a minimum batch thickness of 6 mm(0.25 in.) and
42、pass the stock through the rolls four times,folding it back on itself each time.125TABLE 3 Miniature Internal MixerMixing CycleDuration, min Accumulative, minCharge the mixing chamber with the rubber strips, lowerthe ram, and start the timer.00Masticate the rubber. 1.0 1.0Raise the ram and add zinc
43、oxide, sulfur, stearic acid,and TBBS that have previously been blended, takingcare to avoid any loss. Then add carbon black. Sweepthe orifice and lower the ram.1.0 2.0Allow the batch to mix, raising the ram momentarily tosweep down materials if necessary.7.0 9.0D31870638.6 The precision of these tes
44、t methods may be expressed inthe format of the following 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 associatedTABLE 4 Internal MixerInitial MixDuration, min Accumulative, minAdjust the intern
45、al mixer temperature to achieve thedischarge conditions outlined below. Close thedischarge gate, start the rotor at 8.1 rad/s (77 rpm)and raise the ram.00Charge12 the rubber, all of the zinc oxide, carbonblack, stearic acid, and then the other one half of therubber. Lower the ram.0.53.00.53.0Allow t
46、he batch to mix. 0.5 4.0Raise the ram and clean the mixer throat and the topof the ram. Lower the ram.2.0 6.0Allow the batch to mix until a temperature of 170C(338F) or a total mixing time of 6 min is reached,whichever occurs first. Discharge the batch.00TABLE 5 Internal MixerFinal MixDuration, min
47、Accumulative, minAdjust the internal mixer temperature to 40 6 5C (104 69F), turn off steam and turn on full cooling water to therotors, start the rotors at 8.1 rad/s (77 rpm), and raise theram.00Charge12 the batch, with all the sulfur and accelerator rolledinto this portion of the batch before feed
48、ing to the mixer. Addthe remaining portion of the batch. Lower the ram.0.5 0.5Allow the batch to mix until a temperature of 110 6 5C (2306 9F) or a total mixing time of 3 min is reached, whicheveroccurs first. Discharge the batch.2.5 3.0With the rolls of a standard laboratory mill maintained at 40 6
49、5C (104 6 9F) and set at 0.8 mm (0.032 in.) opening, passthe rolled batch endwise through the rolls six times.2.0 5.0Open the rolls to give a minimum thickness of 6 mm (0.25 in.)and pass the compound through four times, folding it back onitself each time.1.0 6.0TABLE 6 Type 2 Precision for Various Test ParametersNOTESr = Repeatability standard deviation, in measurement units,r = Repeatability, in measurement units,(r) = Repeatability, (relative) percent,SR = Reproducibility standard deviation, in measurement units,R = Reproduc
