1、Designation: D3403 07 (Reapproved 2016)Standard Test Methods forRubberEvaluation of IR (Isoprene Rubber)1This standard is issued under the fixed designation D3403; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last re
2、vision. 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, testformula, mixing procedures, and test methods for the evalua-tion and pro
3、duction control of isoprene rubber (IR).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 theresponsibility of th
4、e 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 Test Methods for RubberVi
5、scosity, 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 PreparingStandard Vulcanized SheetsD3
6、896 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 RubberMeasurement of Unvulca
7、-nized Rheological Properties Using Rotorless Shear Rhe-ometersE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method3. Significance and Use3.1 These tests are mainly intended for referee purposes butmay be used for quality control of rubber production. They
8、may also be used in research and development work and forcomparison of different rubber samples in a standard formula.3.2 These tests may also be used to obtain values forcustomer acceptance of rubber.4. Standard Test Formula4.1 Standard FormulaSee Table 1.5. Sample Preparation5.1 Obtain and prepare
9、 the test samples in accordance withPractice D3896.6. Mixing Procedures6.1 The compound may be prepared in an internal mixer, ona mill, or in a miniature internal mixer. It is not implied thatcomparable results will be obtained. The following mixingprocedures are provided:6.1.1 Method AInternal Mixe
10、r for Initial and FinalMix(6.2),6.1.2 Method BInitial Internal Mix with Final MillMix(6.3),6.1.3 Method CMill Mix, (6.4), and6.1.4 Method DMiniature Internal Mix (6.5).6.2 Internal Mixer for Initial and Final Mix (Method A):6.2.1 For general mixing procedures refer to PracticeD3182.6.2.2 Mixing Cycl
11、e for Internal Mixer Initial Mix (MethodsA,B)See 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 Pass the batch immediately through the standardlaboratory mill three times, with
12、 a mill opening of 6.0 mm(0.25 in.) and roll temperature of 40 6 5C (104 6 9F).6.2.2.3 Allow the batch to rest for 1 to 24 h.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 appr
13、oved June 1, 2016. Published July 2016. Originally approvedin 1975. Last previous edition approved in 2011 as D3403 07 (2011). DOI:10.1520/D3403-07R16.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStan
14、dards 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 19428-2959. United States16.2.3 Mixing Cycle for Internal Mixer Final Mix (MethodA)See Table 3.6.2.3.1 After mixing accord
15、ing to Table 3, measure andrecord the batch mass. If it differs from the theoretical value bymore than 0.5 %, discard the batch.6.2.3.2 If required, cut samples from the batch to allowtesting of compound viscosity and processability in accordancewith Test Methods D1646 or D6204, and vulcanization ch
16、ar-acteristics in accordance with Test Methods D2084 or D5289.6.2.3.3 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 D3182.6.3 Internal Mixer Initial Mix with Final Mill Mix (MethodB):6
17、.3.1 For general mixing procedures, refer to PracticeD3182.6.3.2 Mixing Cycle for Initial MixFollow the procedureoutlined in 6.2.2.6.3.3 Mixing Cycle for Mill Final Mix (Method B)SeeTable 4.6.3.3.1 After mixing according to Table 4, measure andrecord the batch mass. If it differs from the theoretica
18、l value bymore than 0.5 %, discard the batch.6.3.3.2 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.TABLE 1 Standard IR T
19、est FormulaMaterialIRM-SRMNo.AQuantity, Partsby MassIsoprene rubber (IR) . 100.00Zinc oxideA5.00SulfurA2.25Stearic acidA2.00Oil furnace blackBA35.00TBBSCA0.70Total 144.95Batch factor for mill mixD3.00Batch factor for internal mixerD10.00Batch factor for MIM mixE(CamHead)0.50Batch factor for MIM mixE
20、(BanburyHead)0.43AUse current IRM/SRM.BThe current Industry Reference Black (IRB) shall be used.CTBBS is N-tert-butyl-2-benzothiazolesulfenamide.DFor mill and internal mixer batches, weigh the rubber, carbon black, and oil to thenearest 1.0 g, the sulfur and the TBBS accelerator to the nearest 0.02
21、g, and theother compounding materials to the nearest 0.1 g.EFor MIM mixes, weigh the rubber and carbon black to the nearest 0.1 g, thecompounding material blend to the nearest 0.01 g, and the individual compoundingmaterials, if used, to the nearest 0.001 g. For the MIM procedure, it is recom-mended
22、that a blend of compounding materials, excluding carbon black, beprepared to improve the accuracy of the weighing of these materials. This materialblend is prepared by blending a proportional mass of each material in a dry powderblender such as a biconical blender or vee blender. A mortar and pestle
23、 may beused for blending small quantities.TABLE 2 Internal Mixer - Initial CycleDuration,minAccumulative,minAdjust the internal mixer temperature toachieve the discharge conditions outlinedbelow. Close the discharge gate, start therotors at 8.1 rad/s (77 r/min), and raise theram.0.0 0.0Charge one-ha
24、lf of the rubber, all of the zincoxide, carbon black, stearic acid, and thenthe other one-half of the rubber. Lower theram.0.5 0.5Allow the batch to mix. 3.0 3.5Raise the ram, and clean the mixer throatand the top of the ram. Lower the ram.0.5 4.0Allow the batch to mix until a temperature of170C (33
25、8F) or a total of 6 min is reached,whichever occurs first. Discharge the batch.2.0 6.0TABLE 3 Internal Mixer - Final CycleDuration,minAccumulative,minAdjust the internal mixer temperature to 40 5C (104 9F), turn off steam and turn onfull cooling water to the rotors, start the rotorsat 8.1 rad/s (77
26、r/min), and raise the ram.0.0 0.0Charge one-half of the batch, with all thesulfur and accelerator rolled into this portionof the batch before feeding to the mixer. Addthe remaining portion of the batch. Lower theram.0.5 0.5Allow the batch to mix until a temperature of110 5C (230 9F) or a total mixin
27、g timeof 3 min is reached, whichever occurs first.Discharge the batch.2.5 3.0With the rolls of a standard laboratory millmaintained at 40 5C (104 9F), and setat 0.8 mm (0.032 in.) opening, pass the rolledbatch endwise through the mill six times.2.0 5.0Open the rolls to give a minimum thickness of6 m
28、m (0.25 in.) and pass the compoundthrough four times, folding it back on itselfeach time.1.0 6.0TABLE 4 Mill Final Mixing CycleDuration,minAccumulative,minSet the mill opening at 1.90 mm (0.075 in.)and temperature at 70 5C (158 9F).Band the masterbatch on the slow roll.00Add the TBBS accelerator, ta
29、king care toavoid any loss. Sweep the mill pan and adduntil all the accelerator is in the batch. Makethree34 cuts from each side.33Add the sulfur and that which falls into themill pan. Make one34 cut from each side.36Cut the batch from the mill and set the millroll opening at 0.8 mm (0.032 in.). Pas
30、s therolled stock endwise through the mill sixtimes.28Open the mill to give a minimum stockthickness of 6 mm (0.25 in.) and pass thecompound through the mill four times, foldingit back on itself each time.19D3403 07 (2016)26.3.3.3 If tensile stress strain tests are required, sheet off toa finished t
31、hickness of approximately 2.2 mm (0.087 in.) andcondition the compound according to Practice D3182.6.4 Mill Mixing (Method C):6.4.1 For general mixing procedures, refer to PracticeD3182.6.4.2 Mill Mixing CycleSee Table 5.6.4.2.1 After mixing according to Table 5, measure andrecord the batch mass. If
32、 it differs from the theoretical value bymore than 0.5 %, discard the batch.6.4.2.2 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
33、 or D5289.6.4.2.3 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 D3182.6.5 Miniature Internal Mixer (Method D):6.5.1 For general mixing procedures refer to PracticeD3182. Mix with the h
34、ead temperature of the miniatureinternal mixer maintained at 60 6 3C (140 6 5F) and theunloaded rotor speed set at 6.3 to 6.6 rad/s (60 to 63 r/min).6.5.2 Prepare the rubber by passing it through a mill onetime with the temperature set at 70 6 5C (158 6 9F) and anopening that will give a sheet appro
35、ximately 0.5 mm (0.02 in.)thick. Cut the sheet into strips that are approximately 25 mm(1 in.) wide, if desired.6.5.3 MIM Mixing CycleSee Table 6.6.5.3.1 After mixing according to Table 6, turn off themotor, raise the ram, remove the mixing chamber, and dis-charge the batch. Record the maximum batch
36、 temperatureindicated, if desired.6.5.3.2 Immediately pass the discharge from the mixertwice through a standard mill maintained at 70 6 5C (158 69F) 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 endwis
37、e through the mill six timeswith an opening of 0.8 mm (0.032 in.) to enhance thedispersion.6.5.3.3 Measure and record the batch mass. If it differs fromthe theoretical value by more than 0.5 %, discard the batch.TABLE 5 Mill Mixing CycleNOTE 1Do not cut any stock while free carbon black is evident i
38、n the bank or on the milling surface. Be certain to return any materials that dropthrough the mill to the milling stock.Duration,minAccumulative,minWith the mill roll temperature set at 70 5C (158 9F) and the open-ing at 0.20 mm (0.008 in.), pass the rubber through the mill twice withoutbanding.11Se
39、t the mill opening at 1.40 mm (0.056 in.) and band the rubber on theslow roll. Make two34 cuts from each side.23Set the mill opening at 1.70 mm (0.067 in.), add the zinc oxide. Make two34 cuts from each side.25Add the carbon black evenly across the mill at a uniform rate. Whenabout half of the black
40、 is incorporated, add the stearic acid and open themill to 1.90 mm (0.075 in.). Make one34 cut from each side, then add theremainder of the carbon black.14 19Add the TBBS accelerator, taking care to avoid any loss. Sweep the millpan and add until all the accelerator is in the batch. Make three34 cut
41、sfrom each side.322Add the sulfur and that which falls into the mill pan. Make one34 cut fromeach side.5Cut the stock from the mill. Set the opening at 0.8 mm (0.032 in.). Passthe rolled stock endwise through the mill six times.227Open the mill to give a minimum stock thickness of 6 mm (0.25 in.) an
42、dpass the compound through the mill four times, folding it back on itselfeach time.128TABLE 6 Miniature Internal Mixer CycleDuration,minAccumulative,minCharge the mixing chamber with the rubberstrips, lower the ram, and start the timer.0.0 0.0Masticate the masterbatch. 0.5 0.5Raise the ram, and add
43、the previouslyblended zinc oxide, sulfur, stearic acid, andTBBS, taking care to avoid any loss.1.0 1.5Add the carbon black, sweep the orifice, andlower the ram.1.0 2.5Allow the batch to mix, raising the rammomentarily to sweep down, if necessary.6.5 9.0D3403 07 (2016)36.5.3.4 If required, cut sample
44、s 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 D5289.6.5.3.5 If tensile stress strain tests are required, sheet off toa finished thickness of approxim
45、ately 2.2 mm (0.087 in.) andcondition the compound according to Practice D3182.7. Testing Procedures7.1 Cure Meter Measurements of Vulcanization Character-istics:7.1.1 Measure vulcanization characteristics in accordancewith Test Method D2084 (Oscillating Disk Cure MeterMethod) or Test Method D5289 (
46、Rotorless Cure MeterMethod). These methods will not produce equal results.7.1.2 The recommended Test Method D2084 test conditionsare 1.67 Hz (100 cpm) oscillation frequency, 1 oscillationamplitude, 160C die temperature, 30-min test time, and nopreheating. The recommended Test Method D5289 test condi
47、-tions are 1.67 Hz (100 cpm) oscillation frequency, 0.5oscillation amplitude, 160C die temperature, 30-min test time,and no preheating. Test condition tolerances are specified bythe test methods.7.1.3 The recommended standard test parameters are ML,MH,ts1, t50, and t90.7.2 Stress-Strain Measurements
48、 of Vulcanization Character-istics:7.2.1 An alternative to measuring vulcanization character-istics using a cure meter is to prepare and cure test sheets fortensile stress-strain testing.7.2.2 Test sheets shall be prepared and vulcanized in accor-dance with Practice D3182.7.2.3 The recommended stand
49、ard vulcanization times are20, 30, 40, and 60 min at 135C (275F) with the 40-min curepreferred when only one curing time is used.7.2.4 Condition and test tensile specimens for tensile stress,tensile strength, and elongation in accordance with Test Meth-ods D412.NOTE 1Quality control of production may require testing within 1 to6 h to provide close surveillance of the plant operation. In this case,slightly different results may be obtained.8. Precision and Bias38.1 This precision and bias section has been
