1、Designation: D3958 06 (Reapproved 2011)Standard Test Methods forRubberEvaluation of BIIR and CIIR (HalogenatedIsobuteneIsoprene Rubber)1This standard is issued under the fixed designation D3958; the number immediately following the designation indicates the year oforiginal adoption or, in the case o
2、f revision, the 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, testformula, mixing procedures, and test meth
3、ods for the evalua-tion of halogenated isobutene-isoprene rubbers (BIIR andCIIR).1.2 Both mill and miniature internal mixer procedures aregiven.1.3 The values stated in SI units are to be regarded asstandard. The values given in parentheses are for informationonly.1.4 This standard does not purport
4、to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to consult andestablish appropriate safety and health practices and deter-mine the applicability of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standard
5、s:2D412 Test Methods for Vulcanized Rubber and Thermo-plastic ElastomersTensionD1646 Test Methods for RubberViscosity, Stress Relax-ation, and Pre-Vulcanization Characteristics (Mooney Vis-cometer)D2084 Test Method for Rubber PropertyVulcanizationUsing Oscillating Disk Cure MeterD3182 Practice for R
6、ubberMaterials, Equipment, andProcedures for Mixing Standard Compounds and Prepar-ing Standard Vulcanized SheetsD3896 Practice for Rubber From Synthetic SourcesSamplingD4483 Practice for Evaluating Precision for Test MethodStandards in the Rubber and Carbon Black ManufacturingIndustriesD5289 Test Me
7、thod for Rubber PropertyVulcanizationUsing Rotorless Cure MetersD6204 Test Method for RubberMeasurement of Unvul-canized Rheological Properties Using Rotorless ShearRheometers3. Significance and Use3.1 These tests are intended mainly for referee purpose butmay be used for quality control of rubber p
8、roduction. Theymay also be used in research and development work and forcomparison of different samples in a standard formula.3.2 These tests may be used to obtain values for qualitycontrol acceptance of rubber.4. Standard Test Formulas4.1 Standard FormulasSee Table 1.5. Sample Preparation5.1 Obtain
9、 and prepare the test samples in accordance withPractice D3896.6. Mixing Procedures6.1 For general mixing procedures, refer to Practice D3182.6.1.1 The compound may be prepared either on a mill, in aminiature internal mixer, or a lab internal mixer, althoughslightly different results may be obtained
10、.6.2 Mixing Cycles:6.2.1 Method A: Mill MixSee Table 2.6.2.1.1 Mix with the mill roll temperature maintained at 406 5C (104 6 9F). The indicated mill openings should bemaintained insofar as possible to provide a standard foruniform breakdown of the rubber due to milling. Necessaryadjustments may be
11、made to maintain a good working bank atthe nip of the rolls.6.2.1.2 Condition the carbon black in accordance with 5.6of Practice D3182. This is critical with halogenated IIR whenthe simple zinc oxide cure is used.1These test methods are under the jurisdiction of ASTM Committee D11 onRubber and are t
12、he direct responsibility of Subcommittee D11.23 on SyntheticRubbers.Current edition approved Nov. 1, 2011. Published January 2012. Originallyapproved in 1980. Last previous edition approved in 2006 as D3958 06. DOI:10.1520/D3958-06R11.2For referenced ASTM standards, visit the ASTM website, www.astm.
13、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 Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.6.2.1.3 Aft
14、er mixing according to Table 2, measure andrecord the batch mass. If it differs from the theoretical value bymore than 0.5 %, discard the batch.6.2.1.4 If required, cut samples from the batch to allowtesting of compound viscosity and processability in accordancewith Test Methods D1646 or D6204, and
15、vulcanization char-acteristics in accordance with Test Methods D2084 or D5289.6.2.1.5 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 D3182.6.2.2 Method B: Miniature Internal Mixer (MIM)
16、 MixSeeTable 3.6.2.2.1 Mix with the head temperature of the miniatureinternal mixer maintained at 60 6 3C (140 6 5F) and theempty chamber rotor rotational frequency at 1 to 1.05 r/s (60 to63 rpm).6.2.2.2 Condition the carbon black in accordance with 5.6of Practice D3182. This is critical with haloge
17、nated butylrubber when the simple zinc oxide cure is used.6.2.2.3 After mixing according to Table 3, turn off themotor, raise the ram, remove the head, and discharge the batch.Record the batch temperature.6.2.2.4 Immediately pass the discharge from the mixertwice through a standard mill maintained a
18、t 40 6 5C (104 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 mill six timeswith an opening of 0.8 mm (0.31 in.) to enhance the dispersion.6.2.2.5 Measure and record the batch m
19、ass. If it differs fromthe theoretical value by more than 0.5 %, discard the batch.6.2.2.6 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 Method
20、s D2084 or D5289.6.2.2.7 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 Procedure:6.3.1 For general mixing procedure refer to Method D3182.6.3.2 Mixing Cycle-In
21、itial MixSee Table 4.6.3.2.1 After mixing according to Table 4, determine andrecord the batch mass; if the mass differs by more than 0.5 %of the theoretical mass, discard the batch.6.3.2.2 Pass the batch immediately through the standardlaboratory mill three times, set at 6.0 mm (0.25 in.) and 40 65C
22、 (104 6 9F).6.3.2.3 Allow the batch to rest for 1 to 24 h.6.3.3 Final MixSee Table 5.6.3.3.1 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.6.3.3.2 If required, cut samples from the batch to allowtest
23、ing of compound viscosity and processability in accordancewith Test Methods D1646 or D6204, and vulcanization char-acteristics in accordance with Test Methods D2084 or D5289.6.3.3.3 If tensile stress strain tests are required, sheet off toa finished thickness of approximately 2.2 mm (0.087 in.) andc
24、ondition the compound according to Practice D3182.7. Preparation and Testing of Vulcanizates7.1 For tension testing, prepare the test sheets and vulcanizethem in accordance with Practice D3182.7.1.1 The recommended standard cure times for the millmixes are 15, 30, and 45 min at 150C (302F). The reco
25、m-mended cure time for the miniature internal mixer compound is30 min at 150C.7.1.2 Condition the cured sheets for 16 to 96 h at atemperature of 23 6 2C (73 6 3.6F) prior to making tensiontests.NOTE 1Quality control of rubber production may require testingwithin 1 to6htoprovide close surveillance; h
26、owever, slightly differentresults may be obtained.7.1.3 Prepare test specimens and obtain stress at 300 %elongation, tensile stress, and elongation parameters in accor-dance with Test Methods D412.7.2 An alternative to measuring vulcanization characteris-tics by means of tensile stress measurement o
27、n vulcanizates isthe measurement of vulcanization characteristics in accordancewith Test Method D2084 (Oscillating Disk Cure MeterMethod) or Test Method D5289 (Rotorless Cure MeterMethod). These methods will not produce equal results.7.2.1 The recommended Test Method D2084 test conditionsare 1.67 Hz
28、 (100 cpm) oscillation frequency, 1 oscillationamplitude, 160C die temperature, 40-min test time, and nopreheating. The recommended Test Method D5289 test condi-tions are 1.67 Hz (100 cpm) oscillation frequency, 0.5oscillation amplitude, 160C die temperature, 40-min test time,and no preheating. Test
29、 condition tolerances are specified bythe test methods.7.2.2 The recommended standard test parameters are: ML,MH,tsl, t50, and t90.NOTE 2It is recommended that MHbe taken as the torque at 30 min.Where the torque plateaus or peaks before 30 min, MHFor MHR, accordingto the applicable test method, shou
30、ld be used.8. Precision and Bias8.1 This precision and bias section has been prepared inaccordance with Practice D4483. Refer to this practice forterminology and other statistical calculation details.8.1.1 The recommended standard test parameters are ML,MH,tsl, t50, and t90.TABLE 1 Standard Formulas
31、MaterialQuantity Parts byMass FormulaBIIR or CIIR 100.00Zinc oxideA5.00Stearic acidA1.00Current IRB 40.00Total mass 146.00Batch Factors:Mill 2.0BMIM 0.48CAUse current IRM/SRM.BWeigh the rubber and the carbon black to the nearest 0.5 g, the zinc oxide tothe nearest 0.1 g, and the stearic acid to the
32、nearest 0.02 g.CSelect a batch factor for the miniature internal mixer so that the mixingchamber volume will be 75 % filled with stock. A batch factor of 0.48 is suggestedfor the cam blade head with 85-cm3mixing chamber capacity. Calculate all partsto the nearest 0.01 part. Weigh all materials to th
33、e nearest 0.01 g.D3958 06 (2011)28.1.2 Alternate test conditions include use of 3 oscillationamplitude for Test Method D2084 and the use of 1 oscillationamplitude for Test Method D5289. When 3 oscillation ampli-tude is used for Test Method D2084 tests, replace test param-eter ts1with ts2.8.2 The pre
34、cision results in this precision and bias sectiongive an estimate of the precision of this test method 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
35、without documentation that they are applicable tothose particular materials and the specific testing protocols thatinclude this test method.8.3 A Type 2 (interlaboratory) precision was evaluated.Both repeatability and reproducibility are short term, a periodof a few days separates replicate test res
36、ults. For Test MethodD2084 a test result is the value, as specified by this test method,obtained on one determination(s) or measurement(s). For TestMethod D412 a test result is the median of three measurementson separate test pieces.TABLE 2 Method A: Mill MixNOTEDo not cut any stock while free carbo
37、n black is evident in the bank or on the milling surface. Be certain to return any pigments that drop throughthe mill to the milling stock.Duration, min Accumulative, minSet the mill opening at 0.65 mm (0.025 in.)and band the rubber on the slower roll.10Mix the carbon black and the stearic acid anda
38、dd evenly across the mill rolls at a uniformrate. Open the mill nip at intervals to maintaina constant rolling bank. When all the carbonblack has been added, make a34 cut fromeach side.10 11Add the zinc oxide. 3 14Make three34 cuts from each side and cutthe batch from the mill.216Set the mill openin
39、g at 0.8 mm (0.032 in.)and pass the rolled stock end-ways throughthe mill six times.8Total time 18 minTABLE 3 Method B: Miniature Internal Mixer MixDuration, min Accumulative, minCharge the pigments and carbon black first,followed by the rubber cut into approximately20 mm (0.75 in.) wide strips, low
40、er the ram,and start the timing.00Allow the batch to mix, raising the rammomentarily to sweep down, if necessary.5.0 5.0Total time 5.0 minTABLE 4 Mixing CycleInitial MixDuration, min Accumulative, minAdjust the internal mixer temperature to achieve the dischargeconditions outlined below. Close the d
41、ischarge gate, start the rotorat 8.1 rad/s (77 rpm) and raise the ram.00Charge12 the rubber, all of the carbon black and stearic acid, andthen the other one half of the rubber. Lower the ram.0.53.00.53.5Allow the batch to mix. 0.5 4.0Raise the ram and clean the mixer throat and the top of the ram.Lo
42、wer the ram.2.0 6.0Allow the batch to mix until a temperature of 170C (338F) or atotal mixing time of 6 min is reached, whichever occurs first.Discharge the batch.D3958 06 (2011)38.4 Two different materials (rubbers BIIR, CIIR) were usedin the interlaboratory program, these were tested in six labo-r
43、atories on two different days for the internal mixer procedureand in five laboratories on two different days for the millprocedure. The results of the precision calculations for repeat-ability and reproducibility are given in Table 6.8.5 The precision of this test method may be expressed inthe forma
44、t 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 level in Table 6 closest to the mean level underconsideration at any given time for any test and for anymateri
45、al in routine testing operations.8.6 Repeatability The repeatability r, of this test methodhas been established as the appropriate value tabulated in Table6. Two single test results, obtained under normal test methodprocedures, that differ by more than this tabulated r (for anygiven level) must be c
46、onsidered as derived from different ornon-identical sample populations.8.7 ReproducibilityThe reproducibility R, of this testmethod has been established as the appropriate value tabulatedin Table 6. Two single test results obtained in two differentlaboratories, under normal test method procedures, t
47、hat differby more than the tabulated R (for any given level) must beconsidered to have come from different or non-identical samplepopulations.8.8 Repeatability and reproducibility expressed as a per-centage of the mean level, (r) and ( R), have equivalentapplication statements as above for r and R.
48、For the (r) and (R)statements, the difference in the two single test results isexpressed as a percentage of the arithmetic mean of the two testresults.8.9 BiasIn test method terminology, bias is the differencebetween an average test value and the reference (or true) testproperty value. Reference val
49、ues do not exist for this testmethod since the value (of the test property) is exclusivelydefined by the test method. Bias therefore cannot be deter-mined.TABLE 5 Final MixDuration, min Accumulative, minAdjust the internal mixer temperature to 40 6 5C (104 6 9F), turnoff steam and turn on full cooling water to the rotors, start the rotorsat 8.1 rad/s (77 rpm), and raise the ram.Charge12 the batch with all of the zinc oxide rolled into this portionof the batch before feeding into the mixer. Add the remaining portionof the batch.
