1、Designation: D3187 06 (Reapproved 2016)Standard Test Methods forRubberEvaluation of NBR (Acrylonitrile-ButadieneRubber)1This standard is issued under the fixed designation D3187; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the
2、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, testformulas, mixing procedures and test methods for the eval
3、ua-tion of various 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 i
4、s 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 Thermoplas-tic ElastomersTensionD1646
5、Test Methods for RubberViscosity, StressRelaxation, and Pre-Vulcanization Characteristics(Mooney Viscometer)D2084 Test Method for Rubber PropertyVulcanizationUsing Oscillating Disk Cure MeterD3182 Practice for RubberMaterials, Equipment, and Pro-cedures for Mixing Standard Compounds and PreparingSta
6、ndard Vulcanized SheetsD3896 Practice for Rubber From Synthetic SourcesSamplingD4483 Practice for Evaluating Precision for Test MethodStandards in the Rubber and Carbon Black ManufacturingIndustriesD5289 Test Method for Rubber PropertyVulcanizationUsing Rotorless Cure MetersD6204 Test Method for Rub
7、berMeasurement of Unvulca-nized Rheological Properties Using Rotorless Shear Rhe-ometers3. 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 compa
8、rison 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 samp
9、les in accordance with Practice D3896.6. 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 Practice D3182.6.2.1.1
10、 Mix 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
11、CycleSee Table 2.6.2.2.1 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 viscosity and processability in accordancewith Test
12、Methods D1646 or D6204, and vulcanization char-acteristics in accordance with Test Methods D2084 or D5289.1These 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 June 1, 2016.
13、Published July 2016. Originally approvedin 1973. Last previous edition approved in 2011 as D3187 06 (2011). DOI:10.1520/D3187-06R16.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume inform
14、ation, refer to the standards Document Summary page onthe ASTM website.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States16.2.2.3 If tensile stress strain tests are required, sheet off toa finished thickness of approximately 2.2 mm (0.08
15、7 in.) andcondition the compound according to Practice D3182.6.3 Miniature Internal Mixer (MIM) Procedure:6.3.1 For general mixing procedure refer to Practice D3182.6.3.1.1 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
16、rad/s (60 to 63 r/min).6.3.2 Prepare 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
17、3.6.3.3.1 After mixing according 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 6
18、9F) with a roll separation of 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 diffe
19、rs fromthe theoretical value by 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 D1646 or D6204, and vulcanization char-acteristics in accordance with Test Methods D2084 or D5289
20、.6.3.3.5 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 D3182.6.4 Internal Mixer Procedure:6.4.1 For general mixing procedure refer to Practice D3182.6.4.2 Mixing Cycle-Initial MixSee T
21、able 4.6.4.2.1 After mixing 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
22、 Allow the batch to rest for 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 vis
23、cosity and processability in accordancewith Test Methods D1646 or D6204, and vulcanization char-acteristics in accordance with Test Methods D2084 or D5289.6.4.3.3 If tensile stress strain tests are required, sheet off toa finished thickness of approximately 2.2 mm (0.087 in.) andcondition the compou
24、nd according to Practice D3182.7. Preparation and Testing of Vulcanizates7.1 For stress-strain testing, prepare the test sheets andvulcanize them in accordance with Practice D3182.7.1.1 The recommended standard cure times for the millcompound are 20, 40, and 60 min at 150C (302F). Therecommended cur
25、e time for the miniature 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 recom
26、mended standard vulcanization 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
27、specimens and obtain modulus, tensileand elongation parameters in accordance with Test MethodsD412.7.2 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
28、2084 or D5289. These methods will notproduce equal results.7.2.1 The recommended D2084 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 D5289 test conditions are 1.67 Hz oscilla-tion frequenc
29、y, 0.5 oscillation amplitude, 160C dietemperature, 30 min test time, and no preheating. Test condi-tion tolerances are specified by the test methods.7.2.2 The recommended standard test parameters are ML,MH,tsl, t50, and t90.NOTE 3It is recommended that MH, if applicable, be taken as thetorque value
30、at 30 min.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 factor for MIM mix (Banbury Hea
31、d)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, weigh the rubber and carbon
32、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 nearest 0.001 g. For theMIM pro
33、cedure, 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 blender or vee blender. Amort
34、ar and pestle may be used for blending small quantities.D3187 06 (2016)2TABLE 2 Mill Procedure: Mixing CycleNOTE 1Do not cut the batch while free carbon black is evident in the bank or on the milling surface. Be certain to return to the batch any ingredientsthat drop through the mill.Duration, min A
35、ccumulative, 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, without cutting.35Make three34 cuts from each side. 2 7Add half
36、 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 carbon black evenly across the rolls at auniform rate.519When all ca
37、rbon 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 pass the stock through the rolls four times,folding it back on i
38、tself 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 oxide, sulfur, stearic acid,and TBBS that have previously been b
39、lended, 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 9.0TABLE 4 Internal MixerInitial MixDuration, min Accumulative, minAdjust the internal mixer temperature
40、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 the batch to mix. 0.5
41、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.00D3187 06 (2016)38. Precision and Bias8.1 This precision and bias s
42、ection has been prepared inaccordance with Practice D4483. Refer to Practice D4483 forterminology and other statistical calculation details.8.2 The precision results in this precision and bias sectiongive an estimate of the precision of these test methods with thematerials (rubbers) used in the part
43、icular 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 tothose particular materials and the specific testing protocols thatinclude these test methods.8.3 A
44、 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 D412 is the median value, as specified by thesetest methods, obtained on three determination(s) or measure-me
45、nt(s). For Test Methods D1646 and D2084, a test result isobtained from one determination.8.4 Three different materials or rubbers were used in theinterlaboratory program, these were tested in seven laborato-ries on two different days.8.5 The results of the precision calculations for repeatabilityand
46、 reproducibility are given in Table 6.8.6 The precision of these test 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 associatedwith a mean l
47、evel in Table 6 closest to the mean level underconsideration at any given time, for any given material inroutine testing operations.8.7 RepeatabilityThe repeatability, r, of these test meth-ods has been established as the appropriate value tabulated inTABLE 5 Internal MixerFinal MixDuration, min Acc
48、umulative, minAdjust the internal mixer temperature to 40 5C (104 9F),turn off steam and turn on full cooling water to the rotors, startthe rotors at 8.1 rad/s (77 rpm), and raise the ram.00Charge12 the batch, with all the sulfur and accelerator rolledinto this portion of the batch before feeding to
49、 the mixer. Addthe remaining portion of the batch. Lower the ram.0.5 0.5Allow the batch to mix until a temperature of 110 5C (230 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 5C (104 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 i
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