1、Designation: D3182 07 (Reapproved 2012)Standard Practice forRubberMaterials, Equipment, and Procedures for MixingStandard Compounds and Preparing Standard VulcanizedSheets1This standard is issued under the fixed designation D3182; the number immediately following the designation indicates the year o
2、foriginal adoption or, in the case of 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.This standard has been approved for use by agencies of the Department
3、of Defense.1. Scope1.1 This practice provides a listing of reference compound-ing materials required to prepare the rubber test compoundslisted in succeeding methods and contains procedures forweighing. It also specifies the mixing equipment, generalmixing procedures, vulcanization equipment and pro
4、cedures.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 standard to estab
5、lish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. For a specificwarning statement, see 5.5.2. Referenced Documents2.1 ASTM Standards:2D88 Test Method for Saybolt ViscosityD1646 Test Methods for RubberViscosity, Stress Relax-ation,
6、and Pre-Vulcanization Characteristics (Mooney Vis-cometer)D2084 Test Method for Rubber PropertyVulcanizationUsing Oscillating Disk Cure MeterD2161 Practice for Conversion of Kinematic Viscosity toSaybolt Universal Viscosity or to Saybolt Furol ViscosityD2226 Classification for Various Types of Petro
7、leum Oilsfor Rubber Compounding UseD2501 Test Method for Calculation of Viscosity-GravityConstant (VGC) of Petroleum OilsD4678 Practice for RubberPreparation, Testing, Accep-tance, Documentation, and Use of Reference MaterialsD5289 Test Method for Rubber PropertyVulcanizationUsing Rotorless Cure Met
8、ersD6204 Test Method for RubberMeasurement of Unvul-canized Rheological Properties Using Rotorless ShearRheometersE145 Specification for Gravity-Convection and Forced-Ventilation Ovens3. Significance and Use3.1 This practice shall be used for specific procedures usedin preparing rubber compounds for
9、 quality control of produc-tion, for research and development purposes, and for compari-son of different materials.4. Standard Materials4.1 Standard Reference Materials:4.1.1 The materials required for standard rubber test formu-las shall be National Institute of Standards and Technology(NIST) Refer
10、ence Materials or materials that are known tohave properties similar to these standard materials. However,in case of dispute, the following actual standard materials fromthe NIST of the United States shall be used:1This practice is under the jurisdiction ofASTM Committee D11 on Rubber andis the dire
11、ct responsibility of Subcommittee D11.20 on Compounding Materials andProcedures.Current edition approved May 1, 2012. Published May 2012. Originallyapproved in 1973. Last previous edition approved in 2007 as D3182 07. DOI:10.1520/D3182-07R12.2For referenced ASTM standards, visit the ASTM website, ww
12、w.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, PO Box C700, West Conshohocken, PA 19428-2959, United States.4.1.
13、2 An Industry Reference Material (IRM) is a standardreference from a designated supplier and has been certified inaccordance with Practice D4678.3,4Standard IndustryReference ReferenceNIST Standard Reference Material MaterialMaterial or IRM No. No.Zinc oxide 370Sulfur 371Stearic acid 372Benzothiazyl
14、 disulfide 2Tetramethylthiuram disulfide 1Magnesium oxide 376Oil furnace carbon blackHAF 378Gas furnace carbon blackSRF 382Mercaptobenzothiazole 383N-tert-butyl-2-benzothiazolesulfenamide 384SBR-1500 386Natural rubber 2014.2 Other standard or industry reference materials are asfollows: Industry Refe
15、rence Black Current Lot in use at time oftesting ASTM Oil Type 103 (defined by ClassificationD2226).55. Weighing of Materials5.1 The standard batch mass (in grams) for the laboratorymill shall be three times the formula mass in parts per hundredgrams of rubber, unless otherwise specified.5.2 The bat
16、ch mass (in grams) for an internal mixer shall bethe nominal capacity (1170 6 40 cm3) multiplied by thedensity of the rubber compound.5.3 The batch mass (in grams) for a miniature internal mixer(MIM) shall be 75 % of the nominal capacity (85 6 1cm3)multiplied by the density of the rubber compound.5.
17、4 The rubber and carbon black shall be weighed to withina tolerance of 61 g for mill and internal mixer compounds andwith a tolerance of 60.1 g for miniature internal mixercompounds.All other materials shall be weighed with a 60.1-gaccuracy or less for mill and internal mixer compounds andwith 60.01
18、-g accuracy for the miniature internal mixer com-pounds.5.5 Compounding materials other than rubber, carbon black,and oil may be added to miniature internal mixer batches moreprecisely and with greater ease if they are previously blendedin proportion to the mass required by the recipe. Such blendmay
19、 be made in a mortar and pestle, by mixing for 10 min ina biconical blender with intensifier bar turning, or by mixing ina blender6for five 3-s periods and scraping the inside of themixer to dislodge materials stuck to the sides after each 3-smix. (WarningIf mixed longer than 3 s, the stearic acid m
20、aymelt and prevent good dispersion.)5.6 Unless otherwise specified, carbon black shall be con-ditioned by heating for1hat1256 3C (257 6 5F) ina1Boven or equivalent, in accordance with Specification E145.5.6.1 Place the carbon black in an open vessel of suitabledimensions so that the depth of the bla
21、ck is no more than10 mm (0.4 in.) during conditioning. Store the conditionedcarbon black in a closed moisture-proof container until cooland then use for weighing and mixing.6. Equipment for Mixing6.1 Standard Mill:6.1.1 The standard mill shall have rolls between 150 and155 mm (5.9 and 6.1 in.) in di
22、ameter. The mill shall beequipped with retaining guides, with a distance between theguides at the nip of 250 to 280 mm (10 to 11 in.).NOTE 1If mills of other sizes are used, adjustments to batch massesand mixing cycles may be required to obtain equivalent results.6.1.2 The speed of the slow roll sha
23、ll be 0.4 6 0.50 rad/s (246 0.5 rpm) and the ratio between slow and fast roll shall be1:1.4. Other ratios may be used, but modifications in mixingprocedure may be required to obtain equivalent results.The useof other than a standard mill shall be recorded with the reporteddata.6.1.3 Means shall be p
24、rovided for controlling the mill rolltemperatures to the specified temperature 65C (69F).6.1.4 The clearance between rolls shall be adjustable from0.2 to 8.0 mm (0.008 to 0.31 in.) as a minimum range ofadjustment. Roll clearance shall be determined by means oftwo lead strips 10 6 3 mm (0.4 6 0.1 in.
25、) wide, at least 50 mm(2 in.) long, and 0.25 to 0.50 mm (0.01 to 0.02 in.) thicker thanthe roll clearance to be measured. The lead strips shall beinserted, one at each end of the rolls approximately 25 mm(1 in.) from the guides, while a piece of compounded rubber,with Mooney viscosity in excess of 5
26、0 ML 1 + 4 at 100C(212F), approximately 75 by 75 by 6 mm (3 by 3 by 0.25 in.)is passing through the center portion of the rolls. The rolls shallbe at the temperature specified for mixing.After the lead stripshave passed through the rolls, measure the thickness of thestrips to the nearest 0.02 mm (0.
27、001 in.). Tolerance on a rollclearance shall be 610 % or 0.05 mm (0.002 in.), whichever islarger.6.2 Standard Internal MixerThe standard internal mixershall have a chamber of 1575 6 50 cm3volume and two rotorswith approximately 400-cm3displacement volume, resulting in1170 6 40-cm3loading capacity. T
28、he slow rotor speed shall be3NIST has discontinued supply of SRM 373, 374, and 385.Asubstitute materialis available as IRM 2, 1, and 201. The sole source of supply of IRM 1 and 2 knownto the committee at this time is Forcoven Products, Inc., P.O. Box 1556, Humble,TX77338. The sole source of supply o
29、f IRM 201 known to the committee at this timeis Akron Chemical Co., 255 Fountain St., Akron, OH 44304. If you are aware ofalternative suppliers, please provide this information to ASTM InternationalHeadquarters. Your comments will receive careful consideration at a meeting of theresponsible technica
30、l committee,1which you may attend. Supporting data have beenfiled at ASTM International Headquarters and may be obtained by requestingResearch Report RR:D11-1034.4Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D11-1026.5The sole
31、 source of supply of a lot of oil conforming to the basic description inClassification D2226 and, more specifically, to the values listed below known to thecommittee at this time is Sun Refining and Marketing Co., Process Materials Group,10 Penn Center, 1801 Market St., Philadelphia, PA 19103 (avail
32、able in 1 and 5-galquantities): Kinematic Viscosity (Test Method D88) and (Practice D2161) 16.8 61.2 mm2/s at 100F, Viscosity-Gravity Constant (Test Method D2501) 0.889 60.002. If you are aware of alternative suppliers, please provide this information toASTM International Headquarters. Your comments
33、 will receive careful consider-ation at a meeting of the responsible technical committee,1which you may attend.6The sole source of supply of the apparatus known to the committee at this timeis Waring Products, Inc. at . If you are aware ofalternative suppliers, please provide this information to AST
34、M InternationalHeadquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee,1which you may attend.D3182 07 (2012)28.16 rad/s (77 rpm) and the gear ratio shall be 1:1.125. Therotor wing tip to side clearance shall be 2.4 + 0.3, 0.1 mm(0.094 + 0.010
35、, 0.005 in.). The mixer shall be equipped witha thermocouple for measuring and recording batch mixingtemperatures. The thermocouple shall be installed through theend frame and shall protrude into the mixing chamber 25 62.5 mm (1 6 0.1 in.) measured along the top side of thethermocouple probe.Aram th
36、at is 56 6 3mmby1406 8mm(2.2 6 0.1 in. by 5.5 6 0.3 in.) shall exert a force of 1.27 60.06 kN (285 6 14 lbf) on the batch in the chamber. The sidesshall be hinged to swing open, made of cast stainless steel andjacketed for controlling temperature by means of a circulatingliquid or steam. The end fra
37、mes shall be of ductile iron that hasa 0.20 6 0.02-mm (0.008 6 0.001-in.) thick chrome plating onthe working surfaces. Rotors are of stainless steel, nitrided,drilled, and equipped with rotary unions for controlling therotor temperature by means of a circulating liquid or steam.NOTE 2If internal mix
38、ers of other sizes are used, adjustments of batchmasses and rotor speeds or mixing cycles will be required to obtainequivalent results.6.3 Standard Miniature Internal Mixer (MIM):6.3.1 The standard miniature internal mixer shall beequipped with a stainless steel mixer head having a bowl of120-cm3vol
39、ume and stainless steel cam-style mixer rotors(removable or fixed) of 34 to 35-cm3displacement, thusresulting in a 85 6 1-cm3volume. The recommended loadingis 75 % (64 cm3). The fast or driving rotor (left) shall turn at6.28 + 3.14 rad/s (60 + 3, 0 rpm) and the gear ratio (drive todriven) shall be 1
40、.5:1. The mixer shall be equipped with athermocouple installed through the ridge in the bowl formeasuring and recording the batch temperatures. The mixingchamber shall be closed during the mixing cycle by means ofa lever or ram. The head and the backplate shall be maintainedat the required temperatu
41、re either electrically or by means of athermal liquid medium.NOTE 3If miniature internal mixers equipped with Banbury-stylemixer head and rotors or heads of other sizes are used, adjustments ofbatch masses, rotor speeds, or mixing cycles will be required to obtainequivalent results.6.3.2 The miniatu
42、re internal mixer may be equipped with atorque-measuring instrument and recorder, which are notessential for the mixing operation. If used, it must be calibratedoccasionally and after each overhaul of the miniature internalmixer using the manufacturers instructions.7. General Mixing Procedures7.1 Mi
43、ll Mixing Procedure:7.1.1 Mix compounds with the rubber banded on the slowroll, unless otherwise specified.7.1.2 Measure the temperature of the surfaces of the rolls ata point approximately equidistant from the ends during themixing operation either continuously on a recorder or with amanual device
44、having an accuracy of at least 61C (62F),frequently enough to maintain the desired temperature. Thebatch may be removed momentarily from the mill to measurethe surface temperature of the slow roll.7.1.3 Whenever34 cuts are specified, cut the batch34 of thedistance across the roll and hold the knife
45、at this position untilthe bank just disappears. Make successive34 cuts fromalternate ends of the roll, allowing 20 s between each cut unlessotherwise specified.7.1.4 Do not cut any batch while free materials are evidentin the bank or on the milling surface.7.1.5 Add carbon black evenly across the mi
46、ll at a uniformrate. Add all other dry materials slowly and evenly in pre-scribed times. Oil, if required, may be added alternately withcarbon black. Carefully collect materials falling through thenip from the tray and return to the mix.7.1.6 Conclude the mixing cycle by passing the rolled batchendw
47、ise through the mill six times with an opening of 0.8 mm(0.031 in.), to improve the dispersion.7.1.7 Pass the batch four times through the mill at a settingof 6 mm (.25 in.), folding it back on itself each time.7.1.8 Weigh the batch and record the mass. If required, cutsamples from the batch to allo
48、w testing of compound viscosityand processability in accordance with Test Methods D1646 orTest Method D6204, and vulcanization characteristics in ac-cordance with Test Methods D2084 or D5289. If tensile stressstrain tests are required, sheet out the remainder of the batch to2.2 to 2.4 mm (0.087 to 0
49、.094 in.) thickness after shrinkage hastaken place.7.2 Internal Mixer Mixing Procedure:7.2.1 The compound is usually prepared in two stages: thefirst one always in the internal mixer and the second either inthe internal mixer or on the standard mill.7.2.2 The initial internal mixer temperature will be eitherindicated or be such that the required discharge temperature isreached.7.2.3 The rotor speed shall be 8.16 rad/s (77 rpm), unlessotherwise specified.7.2.4 Cut the rubber into pieces suitable for fast feeding.7.2.5 Prepare the
