1、Designation: D 3188 06Standard Test Methods forRubberEvaluation of IIR (Isobutene-Isoprene Rubber)1This standard is issued under the fixed designation D 3188; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revisio
2、n. 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, testformula, mixing procedures, and test methods for the evalua-tion and product
3、ion control of non-halogenated isobutene-isoprene rubbers (IIR), commonly known as butyl rubber.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
4、, associated with its use. It is 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:2D 412 Test Methods for Vulcanized Rubber and Thermo
5、-plastic ElastomersTensionD 1646 Test Methods 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 Mixin
6、g Standard Compounds and Prepar-ing Standard Vulcanized 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 Roto
7、rless Cure MetersD 6204 Test Method for RubberMeasurement of Unvul-canized Rheological Properties Using Rotorless ShearRheometers3. Significance and Use3.1 These test methods are mainly intended for refereepurpose but may be used for quality control of rubber produc-tion. They may also be used in re
8、search and development workand for comparison of different rubber samples in a standardformula.3.2 These test methods may be used to obtain values foracceptance of rubber.4. Standard Test Formula4.1 Standard FormulaSee Table 1.5. Sample Preparation5.1 For tests intended for referee purposes obtain a
9、ndprepare the samples in 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.6.1.1 Method AMill mix (6.2)6.1.2 Method BMiniature Internal Mixer
10、 (MIM) Mix(6.3)6.1.3 Method CLab Banbury (6.4)NOTE 1It is not implied that comparable results will be obtained bythese test methods.6.2 Method AMill Procedure:6.2.1 For general mixing procedures, refer to PracticeD 3182. Mix with the mill roll temperature maintained at 50 65C (122 6 9F). The indicat
11、ed mill openings should bemaintained as nearly as possible to provide a standard degreeof breakdown for the rubber due to milling. Necessary adjust-ments may be made to maintain a good working bank at the nipof the rolls.6.2.2 Mixing CycleSee Table 2.6.2.2.1 After mixing according to Table 2, measur
12、e andrecord the batch mass. If it differs from the theoretical value bymore than 0.5 %, discard the batch.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.
13、 Published March 2006. Originallyapproved in 1973. Last previous edition approved in 2005 as D 3188 05.2For 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
14、 Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.6.2.2.2 If required, cut samples from the batch to allowtesting of compound viscosity and processability in accordancewith Test Methods D 1646
15、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 compound according to Practice D 3182.6.3 Method BMiniature Internal
16、Mixer Mix:6.3.1 For general mixing procedure, refer to PracticeD 3182. Mix with the head temperature of the miniatureinternal mixer maintained at 60 6 3C (140 6 5F) and theunloaded rotor speed at 6.3 to 6.6 rad/s (60 to 63 rpm).6.3.2 Prepare the rubber by passing it through a mill onetime with the t
17、emperature set at 50 6 5C (122 6 9F) and anopening of 0.5 mm (0.02 in.) thick. Cut the sheet into strips thatare approximately 25 mm (1 in.) wide, if desired.6.3.3 Mixing CycleSee Table 3.6.3.3.1 After mixing according to Table 3, turn off themotor, raise the ram, remove the head, and discharge the
18、batch.Measure and record the maximum batch temperature 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 0.5 mm (0.020 in.) once, thentwice at a separation of 3 mm (0.12 in.) in order to dissipatehe
19、at. 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 by more than 0.5 %, discard the batch.6.3.3.4 If required, cut samples from the batch to allow
20、testing 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 strain tests are required, sheet off toa finished thickness of approximately 2.2 mm (0.087 in.)
21、 andcondition the compound according to Practice D 3182.6.4 Internal Mixer Procedure:6.4.1 For general mixing procedure refer to Method D 3182.6.4.2 Mixing Cycle-Initial MixSee Table 4.6.4.2.1 After mixing according to Table 4, measure andrecord the batch mass. If it differs from the theoretical val
22、ue 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 1 to 24 h.6.4.3 Final MixSee Table 5.6.4.3.1 After mixing according to Table 5, measure andre
23、cord 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 accordancewith Test Methods D 1646 or D 6204, and vulcanizationcharacteristics in accordance
24、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 3182.7. Preparation and Testing of Vulcanizates7.1 For stress-strain testing, prepare the test
25、 sheets andvulcanize them in accordance with Practice D 3182.7.1.1 The recommended standard vulcanization time is 40min at 150C (302F).7.1.2 Condition the cured sheets for 16 to 96 h at atemperature of 23 6 2C (73.4 6 3.6F) prior to makingstress-strain tests.NOTE 2Quality control of rubber productio
26、n may require testingwithin 1 to6htoprovide surveillance of the plant operations; however,slightly different results may be obtained.7.1.3 Prepare test specimens and obtain the tensile stress,tension, and elongation in accordance with Test MethodsD 412.8. Testing for Curing Characteristics using Cur
27、e Meters8.1 An alternative to measuring vulcanization characteris-tics by means of tensile stress measurement on vulcanizates isthe measurement of vulcanization characteristics in accordancewith Test Method D 2084 (Oscillating Disk Cure MeterMethod) or Test Method D 5289 (Rotorless Cure MeterMethod)
28、. These methods will not produce equal results.8.1.1 The recommended Test Method D 2084 test condi-tions are 1.67 Hz (100 cpm) oscillation frequency, 1 oscilla-tion amplitude, 160C die temperature, 40-min test time, andno preheating. The recommended Test Method D 5289 testconditions are 1.67 Hz (100
29、 cpm) oscillation frequency, 0.5TABLE 1 Standard FormulaMaterialNBS orIRM No.Quantity, Partsby MassIIR . 100.00Zinc oxideA3.00SulfurA1.75Stearic acidA1.00Oil furnace blackB378 50.00TMTDCA1.00Total mass 156.75Batch factor:MillD2.0Miniature internal mixerECam Head 0.46Banbury Head 0.40AUse current IRM
30、/SRM.BThe current industry reference black may be used in place of NBS 378,although slightly different results may be obtained.CTetramethylthiuram disulfide. NBS has discontinued supply of TMTD. A newsource of supply material is available as IRM 1 from Forcoven Products Inc., P.O.Box 1536, Humble, T
31、X 77338. A research report can be obtained from ASTMHeadquarters. Request RR: D-11-1034.DFor mill mixes, weigh the rubber and carbon black to the nearest 1.0 g, thesulfur and accelerators to the nearest 0.02 g, and all other compounding materialsto the nearest 0.1 g.EFor MIM batches weigh the rubber
32、 carbon black to the nearest 0.1 g, thecompounding material blend to the nearest 0.01 g, and individual compoundingmaterials, if used, to the nearest 0.001 g. For the MIM procedure, it is recom-mended that a blend of compounding materials, including black, be prepared toimprove accuracy in the weigh
33、ing of these materials. This material blend isprepared by blending a proportional mass of each material in a dry powder suchas a biconical blender or vee blender. A mortar and pestle may be used forblending small quantities.D3188062oscillation amplitude, 160C die temperature, 40-min test time,and no
34、 preheating. Test condition tolerances are specified bythe test methods.8.1.2 The recommended standard test parameters are: ML,MH,tsl,t850, and t890.NOTE 3Where the effect of surface contamination is not a problem, a63 angle of oscillation may be used in order to obtain greater sensitivity.In this c
35、ase, the parameter ts2 is to be taken instead of ts1.8.1.3 Alternate test conditions include use of 3 oscillationamplitude for Test Method D 2084 and the use of 1 oscillationamplitude for Test Method D 5289. When 3 oscillationamplitude is used for D 2084 tests, replace test parameter ts1with ts2.NOT
36、E 4It is recommended that MHbe taken as the torque value at 40min.9. Precision and Bias39.1 This precision and bias section has been prepared inaccordance with Practice D 4483. Refer to this practice forterminology and other statistical details.9.2 The precision results in this precision and bias se
37、ctiongive an estimate of the precision of the test method with thematerials used in the particular interlaboratory program as3Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR: D11-1068.TABLE 2 Method AMill Mixing CycleNOTEDo not c
38、ut the batch while free carbon black is evident in the bank or on the milling surface. Be certain to return to the batch any materialsthat drop through the mill.Duration, min Accumulative, minSet the mill opening at 0.65 mm (0.025 in.) and band the rub-ber on the slow roll.11Mix the carbon black and
39、 the stearic acid and add evenlyacross the mill rolls at a uniform rate. Open the mill nip atintervals to maintain a constant rolling bank. When all the car-bon black has been added, make a34 cut from each side.10 11Add all the other materials. 3 14Make three34 cuts from each side and cut the batch
40、from themill.216Set the mill opening at 0.8 mm (0.032 in.) and pass the rolledbatch end-ways through the mill six times.8TABLE 3 Method BMiniature Internal Mixer Mixing CycleDuration, min Accumulative, minCharge the mixing chamber with the rubber strips and theblended materials, lower the ram, and s
41、tart the timer.00Allow to mix. 1 1Raise the ram, add carbon black, sweep the orifice, andlower the ram.12Allow the batch to mix, raising the ram momentarily to sweepdown the materials, if necessary.35TABLE 4 Method CInternal Mixer Initial Mixing CycleDuration, min Accumulative, minAdjust the interna
42、l mixer temperature to achieve the dischargeconditions outlined below. Close the discharge gate, start the rotorat 8.1 rad/s (77 rpm) and raise the ram.00Charge one half the rubber, all of the zinc oxide, carbon black,stearic acid, and then the other one half of the rubber. Lower theram.0.53.00.53.5
43、Allow the batch to mix. 0.5 4.0Raise the ram and clean the mixer throat and the top of the ram.Lower 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.00D3188063described in the following par
44、agraphs. The precision param-eters should not be used for acceptance/rejection testing of anygroup of materials without documentation that they are appli-cable to those particular materials and the specific testingprotocols that include this test method.9.3 A Type 2, Class III interlaboratory precis
45、ion programwas conducted. Materials were tested for ML, MH, ts 2, t50,and t90 using an oscillating disc cure meter. Test MethodD 2084 was followed. Test conditions were as follows:temperature160C; preheatnone; arc63; MHtaken at40 min; oscillation1.7 Hz. Both repeatability and reproduc-ibility are sh
46、ort-term. A period of a few days separates testresults, which were repeated on three separate days. Fourlaboratories participated and three materials were used. There-fore, p =4,q = 3, and n = 3.Atest result is the value obtainedfrom one determination.9.4 The materials used in the test program were
47、isobute-neisoprene rubbers as follows: Polymer A = low Mooney/lowunsaturation; Polymer B = high Mooney/high unsaturation;and Polymer C = low Mooney/high unsaturation. Both rubbersamples and chemicals necessary for the test recipe weredistributed to the participating laboratories.9.5 The results of t
48、he precision calculations for each of theelevated parameters are given in Table 6 with the materialsarranged in increasing mean value within each test type.9.6 The precision of these test methods may be expressed inthe format of the following statements that use what is calledan appropriate value of
49、 r, R, (r), or (R), that is, that value to beused in decisions about test results (obtained with the testmethod). The appropriate value is that value of r or Rassociated with a mean level in Table 6 closest to the meanlevel under consideration at any given time, for any givenmaterial in routine testing operations.9.6.1 RepeatabilityThe repeatability, r, of these test meth-ods has been established as the appropriate value given inTable 6. Two single test results, obtained under normal testmethod procedures, that differ by mo
