1、Designation: D 3403 07Standard Test Methods forRubberEvaluation of IR (Isoprene Rubber)1This standard is issued under the fixed designation D 3403; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number
2、 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, testformula, mixing procedures, and test methods for the evalua-tion and production control
3、 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 the user of this
4、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 for RubberViscosity, Stre
5、ss 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 Vulcanized SheetsD 3896 Pr
6、actice 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 RubberMeasurement of Unvul-cani
7、zed Rheological Properties Using Rotorless ShearRheometersE 691 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. Theymay
8、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 the
9、 test samples in accordance withPractice D 3896.6. 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 Mixer f
10、or Initial and Final Mix(6.2),6.1.2 Method BInitial Internal Mix with Final Mill Mix(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 PracticeD 3182.6.2.2 Mixing Cycle
11、 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 appro
13、ved March 1, 2007. Published April 2007. Originallyapproved in 1975. Last previous edition approved in 2006 as D 3403 06.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refe
14、r 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.6.2.3 Mixing Cycle for Internal Mixer Final Mix (MethodA)See Table 3.6.2.3.1 After mixing according to Table 3, measure andre
15、cord 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 D 1646 or D 6204, and vulcanizationcharacteristics in accordance
16、with Test Methods D 2084 orD 5289.6.2.3.3 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 D 3182.6.3 Internal Mixer Initial Mix with Final Mill Mix (MethodB):6.3.1 For general mixing pro
17、cedures, refer to PracticeD 3182.6.3.2 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 theoretical value bymore than 0.5 %,
18、 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 D 1646 or D 6204, and vulcanizationcharacteristics in accordance with Test Methods D 2084 orD 5289.TABLE 1 Standard IR Test FormulaMaterialIRM-SR
19、MNo.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(BanburyHead)0.43AUse cur
20、rent 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 tothe nearest 1.0 g, the sulfur and the TBBS accelerator to the nearest 0.02 g, andthe other compoundi
21、ng 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 that a blend of compoundi
22、ng 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 may beused for blending
23、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-half of the rubber, all of
24、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 (338F) or a total of 6 min i
25、s reached,whichever occurs first. Discharge the batch.2.0 6.0TABLE 3 Internal Mixer - Final CycleDuration,minAccumulative,minAdjust the internal mixer temperature to 40 65C (104 6 9F), turn off steam and turn onfull cooling water to the rotors, start the rotorsat 8.1 rad/s (77 r/min), and raise the
26、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 6 5C (230 6 9F) or a total mixing timeof 3 min is
27、reached, whichever occurs first.Discharge the batch.2.5 3.0With the rolls of a standard laboratory millmaintained at 40 6 5C (104 6 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 mm (0.25 in.) a
28、nd 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 6 5C (158 6 9F).Band the masterbatch on the slow roll.00Add the TBBS accelerator, taking care
29、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.). Pass therolle
30、d 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.19D34030726.3.3.3 If tensile stress strain tests are required, sheet off toa finished thickness of approx
31、imately 2.2 mm (0.087 in.) andcondition the compound according to Practice D 3182.6.4 Mill Mixing (Method C):6.4.1 For general mixing procedures, refer to PracticeD 3182.6.4.2 Mill Mixing CycleSee Table 5.6.4.2.1 After mixing according to Table 5, measure andrecord the batch mass. If it differs from
32、 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 D 1646 or D 6204, and vulcanizationcharacteristics in accordance with Test Methods D 2084 orD 5289.6.4.2
33、.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 3182.6.5 Miniature Internal Mixer (Method D):6.5.1 For general mixing procedures refer to PracticeD 3182. Mix with the head temperatu
34、re 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 approximately 0.5
35、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 temperaturei
36、ndicated, 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 endwise through the
37、 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 CycleNOTEDo not cut any stock while free carbon black is evident in the bank or o
38、n the milling surface. Be certain to return any materials that drop throughthe mill to the milling stock.Duration,minAccumula-tive,minWith the mill roll temperature set at 70 6 5C (158 6 9F) and the open-ing at 0.20 mm (0.008 in.), pass the rubber through the mill twice withoutbanding.11Set the mill
39、 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 is incorp
40、orated, 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 cutsfrom each
41、 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.) andpass the
42、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 the previo
43、uslyblended 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 9.0D34030736.5.3.4 If required, cut samples from the batch t
44、o 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 5289.6.5.3.5 If tensile stress strain tests are required, sheet off toa finished thickness of approximately 2.2 mm (0.0
45、87 in.) andcondition the compound according to Practice D 3182.7. Testing Procedures7.1 Cure Meter Measurements of Vulcanization Character-istics:7.1.1 Measure vulcanization characteristics in accordancewith Test Method D 2084 (Oscillating Disk Cure MeterMethod) or Test Method D 5289 (Rotorless Cure
46、 MeterMethod). These methods will not produce equal results.7.1.2 The recommended Test Method D 2084 test condi-tions are 1.67 Hz (100 cpm) oscillation frequency, 1 oscilla-tion amplitude, 160C die temperature, 30-min test time, andno preheating. The recommended Test Method D 5289 testconditions are
47、 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,t850, and t890.7.2 Stress-Strain Measurements of Vulca
48、nization 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 D 3182.7.2.3 The recommended standard vulc
49、anization 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 D 412.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 prepared inaccordance with Prac
