1、Designation: D 3184 07Standard Test Methods forRubberEvaluation of NR (Natural Rubber)1This standard is issued under the fixed designation D 3184; 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, testformulas, mixing procedures, and test methods for the evalu-ation and production control
3、 of natural rubber (NR).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 s
4、tandard 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 1485 Test Methods for Rubber from Natural So
5、urcesSampling and Sample PreparationD 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
6、 for Mixing Standard Compounds and Prepar-ing Standard Vulcanized SheetsD 4483 Practice for Evaluating Precision for Test MethodStandards in the Rubber and Carbon Black ManufacturingIndustries3. Significance and Use3.1 These tests are mainly intended for referee purposes butmay be used for quality c
7、ontrol of rubber production. Theymay also be used in research and development work and forcomparison of different rubber samples in a standard formula.4. Standard Test Formulas4.1 Standard Formulas:Quantity, Parts by Mass, and Formula No.MaterialIndustryReferenceMaterial No.1A Gum 2A BlackFilled3AAG
8、umNatural rubber . 100.00 100.00 100.00Zinc oxide 091 6.00 5.00 6.00Sulfur 031 3.50 2.25 3.50Stearic acid 021 0.50 2.00 0.50Oil furnaceblackBIRB#7 . 35.00 .Mercaptoben-zothiazole002 0.50 . .TBBSC003 . 0. 70 0.70Total 110.50 144.95 110.70Batch factor:DMill 3.0 3.0 3.0Miniature internalmixer:ECam Head
9、 0.57 0.48 0.57Banbury Head 0.50 0.42 0.50ARecommended formula for Test Method D 2084 vulcanization characteristicsusing oscillating disk cure meter.BThe current Industry Reference Black may be used in place of NIST 378,although slightly different results may be obtained.CN-tert-butyl-2-benzothiazol
10、e sulfenamide.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 carbon black to the nearest 0.1 g, thecompounding material blend to the n
11、earest 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 weighing of these materials. This material blend is pre-pared by blending a pro
12、portional mass of each material in a dry powder such as abiconical blender or vee blender. A mortar and pestle may be used for blendingsmall quantities.5. Sample Preparation5.1 For tests intended for referee purposes obtain andprepare the samples in accordance with Test Methods D 1485.6. Mixing Proc
13、edures6.1 The following three mixing procedures are offered asfollows:6.1.1 Mill Method AFor gum formulas 1A and 3A.6.1.2 Mill Method BFor black formula 2A.6.1.3 MIM Method CFor formula 1A, 2A, and 3A.NOTE 1It is not implied that comparable results will be obtained bythese test methods.6.2 Mill Meth
14、od A:1These test methods are under the jurisdiction of ASTM Committee D11 onRubber and are the direct responsibility of Subcommittee D11.22 on NaturalRubber.Current edition approved March 1, 2007. Published April 2007. Originallyapproved in 1973. Last previous edition approved in 2001 as D 3184 89 (
15、2001).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.1Copyright ASTM International, 100 Barr Harbor Drive, P
16、O Box C700, West Conshohocken, PA 19428-2959, United States.6.2.1 For general mixing procedures, refer to PracticeD 3182.6.2.2 Mixing shall be done with the mill roll temperaturemaintained at 70 6 5C (158 6 9F). The indicated millopenings are desired and should be maintained insofar aspossible to pr
17、ovide a standard for uniform breakdown of therubber due to milling.6.2.3 Mixing CycleGum Compound:Dura-tion,minAccumu-lative,minSet the mill opening at 0.20 mm (0.008 in.) and pass therubber through the rolls twice without banding.11Band with the mill opening at 1.40 mm (0.055 in.) andbreak down, op
18、ening the mill to 1.90 mm (0.075 in.) asthe band becomes smooth.45Add the stearic acid. 2 7Add the zinc oxide, sulfur, and accelerator. 4 11Make three34 cuts from each side. 2 13Cut the stock from the mill. Set the opening at 0.80 mm(0.032 in.) and pass the rolled stock endwise through themill six t
19、imes.215Open the mill to give a minimum stock thickness of 6mm (0.25 in.) and pass the stock through the rolls fourtimes, folding it back on itself each time.318_ _Total Time 186.2.3.1 Check the batch mass and record. If it differs fromthe theoretical value by more than 0.5 %, reject the batch.6.2.3
20、.2 From this stock, cut enough sample to allow testingof compounded viscosity in accordance with Test MethodsD 1646 or curing characteristics in accordance with TestMethod D 2084, or both, if these are desired. Sheet off thestock from the mill at a setting to give an approximate finishgage of 2.2 mm
21、 (0.085 in.). Cool on a flat, dry metal surface.6.2.3.3 For routine laboratory testing, condition the sheetedcompound for 1 to 24 h at 23 6 2C (73.4 6 3.6F) and arelative humidity not greater than 55 %. For maximum preci-sion, condition for 1 to 24 h in a closed container to preventabsorption of moi
22、sture from the air or in an area controlled at35 6 5 % relative humidity.6.3 Mill Method B:6.3.1 For general mixing procedures, refer to PracticeD 3182.6.3.2 Mixing shall be done with the mill roll temperaturemaintained at 70 6 5C (158 6 9F). The indicated millopenings are desired and should be main
23、tained insofar aspossible to provide a standard for uniform breakdown of therubber due to milling.6.3.3 Mixing CycleBlack-Filled Compound:Dura-tion,minAccumu-lative,minSet the mill opening at 0.20 mm (0.008 in.) and pass therubber through the rolls twice without banding.11Band the rubber on the fron
24、t roll with the mill opening at1.40 mm (0.055 in.). Make two34 cuts from each side.23NOTEDo not cut any stock while free carbon black is evident in thebank or on the milling surface. Be certain to run any pigments that dropthrough the mill to the milling stock.Dura-tion,minAccumu-lative,minSet the m
25、ill opening at 1.70 mm (0.067 in.). Add zincoxide. Make one34 cut from each side.25Add the carbon black evenly across the mill at a uniformrate. When about half the black is incorporated, add thestearic acid and open the mill to 1.90 mm (0.075 in.).Make one34 cut from each side then add the remainde
26、rof the carbon black.14 19Add the accelerator, taking care to avoid any loss.Sweep the mill pan and add until all the pigment is in thebatch. Make three34 cuts from each side.221Add the sulfur and that which falls into the mill pan.Make one34 cut from each side.324Cut the stock from the mill. Set th
27、e opening at 0.80 mm(0.032 in.) and pass the rolled stock endwise through themill six times.226Open the mill to give a minimum stock thickness of 6mm (0.25 in.) and pass the stock through the rolls fourtimes, folding it back on itself each time.329_ _Total Time 296.3.3.1 Check the batch mass and rec
28、ord. If it differs fromthe theoretical value by more than 0.5 % reject the batch.6.3.3.2 From this stock, cut enough sample to allow testingof compounded viscosity in accordance with Test MethodsD 1646, or curing characteristics in accordance with TestMethod D 2084, or both, if these are desired. Sh
29、eet off thestock from the mill at a setting to give an approximate finishgage of 2.20 mm (0.085 in.). Cool on a flat, dry metal surface.6.3.3.3 For routine laboratory testing, condition the sheetedcompound for 1 to 24 h at 23 6 2C (73.4 6 3.6F) and arelative humidity not greater than 55 %. For maxim
30、um preci-sion, condition for 1 to 24 h in a closed container to preventabsorption of moisture from the air or in an area controlled at35 6 5 % relative humidity.6.4 Method CMiniature Internal Mixer Mix:6.4.1 For general mixing procedure, refer to PracticeD 3182. Mix with the head temperature of the
31、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).6.4.2 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 tha
32、tare approximately 25 mm (1 in.) wide if desired.6.4.3 Mixing Cycle:Dura-tion,minAccumu-lative,minCharge the mixing chamber with the rubber strips 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.12Al
33、low the batch to mix, raising the ram momentarily tosweep down the materials, if necessary.356.4.3.1 Turn off the motor, raise the ram, remove the headand discharge the batch. Measure and record the maximumbatch temperature if desired.D31840726.4.3.2 Immediately pass the batch twice through a labora
34、-tory mill maintained at 50 6 5C (122 6 9F) and with the rollseparation of 3 mm (0.125 in.).6.4.3.3 Check the batch mass and record. If it differs fromthe theoretical value by more than 0.5 %, discard the batch.6.4.3.4 Cut a specimen for testing vulcanization character-istics in accordance with Test
35、 Method D 2084, if required.Condition the specimen for 1 to 24 h at 23 6 3C (73.4 65.4F) before testing.6.4.3.5 If either compound viscosity or stress-strain testingis required, pass the rolled compound end-wise through themill six times with the mill rolls set at 50 6 5C (122 6 9F)and 0.8 mm (0.032
36、 in.).6.4.3.6 Cut a specimen to allow testing for compoundviscosity in accordance with Test Methods D 1646, if required.6.4.3.7 If tensile stress is required, sheet off the compoundfrom the mill at a setting to give a finished gage of approxi-mately 2.2 mm (0.085 in.) by passing the folded stock bet
37、weenthe rolls set at 50 6 5C (122 6 9F) four times always in thesame direction to obtain the effects of mill direction. Cool ona flat, dry metal surface.6.4.3.8 For routine laboratory testing, condition the sheetedcompound for 1 to 24 h at 23 6 3C (73.4 6 5.4F) and arelative humidity not greater tha
38、n 55 %. For maximum preci-sion, condition for 1 to 24 h in a closed container to preventabsorption of moisture from the air or in an area controlled at35 6 5 % relative humidity.7. Preparation and Testing of Vulcanizates7.1 For stress-strain testing, prepare test slabs and vulcanizethem in accordanc
39、e with Practice D 3182.7.1.1 The recommended standard cure times are 10, 20, 40,and 80 min at 140C (284F).7.1.2 Condition the cure sheets for 16 to 96 h at a tempera-ture of 23 6 2C (73.4 6 3.6F).NOTE 2Quality control of production may require testing within 1 to6 h, to provide close surveillance of
40、 the plant operations; however, slightlydifferent results may be obtained.7.1.3 Prepare test specimens in accordance with PracticeD 3182 and obtain modulus, tensile, and elongation parametersin accordance with Test Methods D 412.7.2 An alternative to measuring stress-strain properties ofvulcanizates
41、 is the cure meter measurement of vulcanizationparameters in accordance with Test Method D 2084.7.2.1 The recommended standard test conditions are 1.7 Hz(100 cpm) oscillation frequency, 1 6 0.03 amplitude ofoscillation, and 160 6 0.3C (320 6 0.5F) die temperature.7.2.2 The recommended standard test
42、parameters are ML,MH, tS1, t8 (50), and t8 (90). For formula 3A, use MHFinsteadof MH.8. Precision and Bias8.1 Precision and bias statements are in the process of beingprepared as prescribed in Practice D 4483. They will be addedto this test method when they are completed.9. Keywords9.1 mill method;
43、miniature mixer; mixing procedures; natu-ral rubber; sample preparation; test methodsASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of th
44、e validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. You
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46、 have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).D3184073
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