1、Designation: D3188 06 (Reapproved 2017)Standard Test Methods forRubberEvaluation of IIR (Isobutene-Isoprene Rubber)1This standard is issued under the fixed designation D3188; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year
2、 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 methods for the evalua-t
3、ion and production 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 c
4、oncerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety, health, and environmental practices and deter-mine the applicability of regulatory limitations prior to use.1.4 This international standard was developed in accor-dance wi
5、th internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standard
6、s:2D412 Test Methods for Vulcanized Rubber and Thermoplas-tic ElastomersTensionD1646 Test Methods for RubberViscosity, StressRelaxation, and Pre-Vulcanization Characteristics(Mooney Viscometer)D2084 Test Method for Rubber PropertyVulcanizationUsing Oscillating Disk Cure MeterD3182 Practice for Rubbe
7、rMaterials, Equipment, and Pro-cedures for Mixing Standard Compounds and PreparingStandard Vulcanized SheetsD3896 Practice for Rubber From Synthetic SourcesSamplingD4483 Practice for Evaluating Precision for Test MethodStandards in the Rubber and Carbon Black ManufacturingIndustriesD5289 Test Method
8、 for Rubber PropertyVulcanizationUsing Rotorless Cure MetersD6204 Test Method for RubberMeasurement of Unvulca-nized Rheological Properties Using Rotorless Shear Rhe-ometers3. Significance and Use3.1 These test methods are mainly intended for refereepurpose but may be used for quality control of rub
9、ber produc-tion. They may also be used in research 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
10、tests intended for referee purposes obtain andprepare the samples 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.6.1.1 Method AMill mix
11、(6.2)6.1.2 Method BMiniature Internal Mixer (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 PracticeD3182. Mix with the mill roll temperature m
12、aintained at 50 65C (122 6 9F). The indicated 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 2.1These
13、 test methods are under the jurisdiction of ASTM Committee D11 onRubber and Rubber-like Materials and are the direct responsibility of SubcommitteeD11.23 on Synthetic Rubbers.Current edition approved Oct. 1, 2017. Published December 2017. Originallyapproved in 1973. Last previous edition approved in
14、 2010 as D3188 06 (2010).DOI: 10.1520/D3188-06R17.2For 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 Document Summary page onthe ASTM website.Copyright A
15、STM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International St
16、andards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.16.2.2.1 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
17、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 D5289.6.2.2.3 If tensile stress strain tests are required, sheet off toa finished thickness of ap
18、proximately 2.2 mm (0.087 in.) andcondition the compound according to Practice D3182.6.3 Method BMiniature Internal Mixer Mix:6.3.1 For general mixing procedure, refer to PracticeD3182. Mix with the head temperature of the miniatureinternal mixer maintained at 60 6 3C (140 6 5F) and theunloaded roto
19、r 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 temperature 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
20、 3.6.3.3.1 After mixing according to Table 3, turn off themotor, raise the ram, remove the head, and discharge the 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
21、 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 differs fromt
22、he 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 D5289.6.3.3.5
23、 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 Method D3182.6.4.2 Mixing Cycle-Initial MixSee Table 4.6.4
24、.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 Allow the
25、 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 viscosity and
26、 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 compound accordi
27、ng 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 vulcanization time is 40min at 150C (302F).7.1.2 Condition the cured sheets for 16 to 96 h at atemp
28、erature of 23 6 2C (73.4 6 3.6F) prior to makingstress-strain tests.NOTE 2Quality control of rubber production 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
29、,tension, and elongation in accordance with Test MethodsD412.8. Testing for Curing Characteristics using Cure Meters8.1 An alternative to measuring vulcanization characteris-tics by means of tensile stress measurement on vulcanizates isthe measurement of vulcanization characteristics in accordancewi
30、th Test Method D2084 (Oscillating Disk Cure MeterMethod) or Test Method D5289 (Rotorless Cure MeterMethod). These methods will not produce equal results.8.1.1 The recommended Test Method D2084 test conditionsare 1.67 Hz (100 cpm) oscillation frequency, 1 oscillationamplitude, 160C die temperature, 4
31、0-min test time, and nopreheating. The recommended Test Method D5289 test condi-tions are 1.67 Hz (100 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 m
32、ass 156.75Batch factor:MillD2.0Miniature internal mixerECam Head 0.46Banbury Head 0.40AUse current IRM/SRM.BThe current industry reference black may be used in place of NBS 378, althoughslightly different results may be obtained.CTetramethylthiuram disulfide. NBS has discontinued supply of TMTD. A n
33、ewsource of supply material is available as IRM 1 from Forcoven Products Inc., P.O.Box 1536, Humble, TX 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, the sulfurand accelerators to the nea
34、rest 0.02 g, and all other compounding materials to thenearest 0.1 g.EFor MIM batches weigh the rubber 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-mend
35、ed that a blend of compounding materials, including black, be prepared toimprove accuracy in the weighing 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 for
36、blending small quantities.D3188 06 (2017)2oscillation amplitude, 160C die temperature, 40-min test time,and no preheating. Test condition tolerances are specified bythe test methods.8.1.2 The recommended standard test parameters are: ML,MH,tsl, t50, and t90.NOTE 3Where the effect of surface contamin
37、ation is not a problem, a63 angle of oscillation may be used in order to obtain greater sensitivity.In this case, the parameter ts2 is to be taken instead of ts1.8.1.3 Alternate test conditions include use of 3 oscillationamplitude for Test Method D2084 and the use of 1 oscillationamplitude for Test
38、 Method D5289. When 3 oscillation ampli-tude is used for D2084 tests, replace test parameter ts1with ts2.NOTE 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 D4483. Refer to this pr
39、actice forterminology and other statistical details.9.2 The precision results in this precision and bias sectiongive an estimate of the precision of the test method with the3Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D11-106
40、8.TABLE 2 Method AMill 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 materialsthat drop through the mill.Duration, min Accumulative, minSet the mill opening at 0.65 mm (0.025 in.) and band the ru
41、b-ber on the slow roll.11Mix the carbon black and 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 14Ma
42、ke three34 cuts from each side and cut the batch 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 stri
43、ps and theblended materials, lower the ram, and start 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 Cycle
44、Duration, min Accumulative, minAdjust the internal mixer temperature toachieve the discharge conditions outlinedbelow. Close the discharge gate, start therotor at 8.1 rad/s (77 rpm) and raise the ram.00Charge one half the rubber, all of the zincoxide, carbon black, stearic acid, and then theother on
45、e 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 andthe top of the ram. Lower the ram.2.0 6.0Allow the batch to mix until a temperature of170C (338F) or a total mixing time of 6 minis reached, whichever occurs first. Dischargethe
46、 batch.00D3188 06 (2017)3materials used in the particular interlaboratory program asdescribed in the following paragraphs. 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 materi
47、als and the specific testingprotocols that include this test method.9.3 A Type 2, Class III interlaboratory precision programwas conducted. Materials were tested for ML, MH, ts2, t50, andt90 using an oscillating disc cure meter. Test Method D2084was followed. Test conditions were as follows: tempera
48、ture160C; preheatnone; arc63; MHtaken at 40 min;oscillation1.7 Hz. Both repeatability and reproducibility areshort-term. A period of a few days separates test results, whichwere repeated on three separate days. Four laboratories par-ticipated and three materials were used. Therefore, p =4,q= 3, and
49、n = 3. A test result is the value obtained from onedetermination.9.4 The materials used in the test program were 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 the precision calculations for each of theelevated parameters are given in Table 6 with the materialsarranged in
