1、Designation: D3182 15D3182 15aStandard 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 oforiginal
2、 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 U.S. Department of D
3、efense.1. Scope1.1 This practice provides a listing of reference compounding materials required to prepare the rubber test compounds listed insucceeding methods and contains procedures for weighing. It also specifies the mixing equipment, general mixing procedures,vulcanization equipment and procedu
4、res.1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establ
5、ish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use. For a specific warning statement, see 5.5.2. Referenced Documents2.1 ASTM Standards:2D88 Test Method for Saybolt ViscosityD1646 Test Methods for RubberViscosity, Stress Relaxation, and
6、Pre-Vulcanization Characteristics (Mooney Viscometer)D2084 Test Method for Rubber PropertyVulcanization Using Oscillating Disk Cure MeterD2161 Practice for Conversion of Kinematic Viscosity to Saybolt Universal Viscosity or to Saybolt Furol ViscosityD2226 Classification for Various Types of Petroleu
7、m Oils for Rubber Compounding UseD2501 Test Method for Calculation of Viscosity-Gravity Constant (VGC) of Petroleum OilsD4678 Practice for RubberPreparation, Testing, Acceptance, Documentation, and Use of Reference MaterialsD5289 Test Method for Rubber PropertyVulcanization Using Rotorless Cure Mete
8、rsD6204 Test Method for RubberMeasurement of Unvulcanized Rheological Properties Using Rotorless Shear RheometersE145 Specification for Gravity-Convection and Forced-Ventilation Ovens3. Significance and Use3.1 This practice shall be used for specific procedures used in preparing rubber compounds for
9、 quality control of production,for research and development purposes, and for comparison of different materials.4. Standard Materials4.1 Standard Reference Materials:4.1.1 The materials required for standard rubber test formulas shall be National Institute of Standards and Technology (NIST)Reference
10、 Materials or materials that are known to have properties similar to these standard materials. However, in case of dispute,the following actual standard materials from the NIST of the United States shall be used:1 This practice is under the jurisdiction of ASTM Committee D11 on Rubber and is the dir
11、ect responsibility of Subcommittee D11.20 on Compounding Materials andProcedures.Current edition approved June 1, 2015July 15, 2015. Published July 2015October 2015. Originally approved in 1973. Last previous edition approved in 20122015 asD3182 07 (2012).D3182 15. DOI: 10.1520/D3182-15.10.1520/D318
12、2-15A.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.This document is not an ASTM standard and is intended o
13、nly to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current ver
14、sionof the standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States14.1.2 An Industry Reference Material (IRM) is a standard reference from a designated supplier and has b
15、een certified inaccordance with Practice D4678.3,4Standard IndustryReference ReferenceNIST Standard Reference Material MaterialMaterial or IRM No. No.Zinc oxide 370Sulfur 371Stearic acid 372Benzothiazyl disulfide 2Tetramethylthiuram disulfide 1Magnesium oxide 376Oil furnace carbon blackHAF 378Gas fu
16、rnace carbon blackSRF 382Mercaptobenzothiazole 383N-tert-butyl-2-benzothiazolesulfenamide 384SBR-1500 386Natural rubber 2014.2 Other standard or industry reference materials are as follows: Industry Reference Black Current Lot in use at time of testingASTM Oil Type 103 (defined by Classification D22
17、26).55. Weighing of Materials5.1 The standard batch mass (in grams) for the laboratory mill shall be three times the formula mass in parts per hundred gramsof rubber, unless otherwise specified.5.2 The batch mass (in grams) for an internal mixer shall be the nominal capacity (1170 6 40 cm3) multipli
18、ed by the densityof 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 1 cm3)multiplied by the density of the rubber compound.5.4 The rubber and carbon black shall be weighed to within a tolerance of61 g for mill and int
19、ernal mixer compounds and witha tolerance of 60.1 g for miniature internal mixer compounds.All other materials shall be weighed with a 60.1-g accuracy or lessfor mill and internal mixer compounds and with 60.01-g accuracy for the miniature internal mixer compounds.5.5 Compounding materials other tha
20、n rubber, carbon black, and oil may be added to miniature internal mixer batches moreprecisely and with greater ease if they are previously blended in proportion to the mass required by the recipe. Such blend maybe made in a mortar and pestle, by mixing for 10 min in a biconical blender with intensi
21、fier bar turning, or by mixing in a blender6for five 3-s periods and scraping the inside of the mixer to dislodge materials stuck to the sides after each 3-s mix. (WarningIf mixed longer than 3 s, the stearic acid may melt and prevent good dispersion.)5.6 Unless otherwise specified, carbon black sha
22、ll be conditioned by heating for 1 h at 125 6 3C (257 6 5F) in a 1 B ovenor equivalent, in accordance with Specification E145.5.6.1 Place the carbon black in an open vessel of suitable dimensions so that the depth of the black is no more than 10 mm (0.4in.) during conditioning. Store the conditioned
23、 carbon black in a closed moisture-proof container until cool and then use forweighing and mixing.6. Equipment for Mixing6.1 Standard Mill:6.1.1 The standard mill shall have rolls between 150 and 155 mm (5.9 and 6.1 in.) in diameter. The mill shall be equipped withretaining guides, with a distance b
24、etween the guides at the nip of 250 to 280 mm (10 to 11 in.).NOTE 1If mills of other sizes are used, adjustments to batch masses and mixing cycles may be required to obtain equivalent results.3 NIST has discontinued supply of SRM 373, 374, and 385. A substitute material is available as IRM 2, 1, and
25、 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, TX 77338. The sole source of supply of IRM 201 known to the committee at this timeis Akron Chemical Co., 255 Fountain St., Akron, OH 44304. If you are aware of alterna
26、tive suppliers, please provide this information to ASTM International Headquarters.Your comments will receive careful consideration at a meeting of the responsible technical committee,1 which you may attend. Supporting data have been filed at ASTMInternational Headquarters and may be obtained by req
27、uesting Research Report RR:D11-1034.4 Supporting data have been filed at ASTM International Headquarters and may be obtained by requesting Research Report RR:D11-1026.5 The sole source of supply of a lot of oil conforming to the basic description in Classification D2226 and, more specifically, to th
28、e 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 (available in 1 and 5-galquantities): Kinematic Viscosity (Test Method D88) and (Practice D2161) 16.8 6 1.2 mm2/s at 100F, Visc
29、osity-Gravity Constant (Test Method D2501) 0.889 6 0.002. Ifyou are aware of alternative suppliers, please provide this information to ASTM International Headquarters. Your comments will receive careful consideration at a meetingof the responsible technical committee,1 which you may attend.6 The sol
30、e source of supply of the apparatus known to the committee at this time is Waring Products, Inc. at . If you are aware of alternativesuppliers, please provide this information to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the responsible technic
31、alcommittee,1 which you may attend.D3182 15a26.1.2 The speed of the slow roll shall be 0.4 6 0.50 rad/s (24 6 0.5 rpm) and the ratio between slow and fast roll shall be 1:1.4.Other ratios may be used, but modifications in mixing procedure may be required to obtain equivalent results. The use of othe
32、rthan a standard mill shall be recorded with the reported data.6.1.3 Means shall be provided for controlling the mill roll temperatures to the specified temperature 65C (69F).6.1.4 The clearance between rolls shall be adjustable from 0.2 to 8.0 mm (0.008 to 0.31 in.) as a minimum range of adjustment
33、.Roll clearance shall be determined by means of two lead strips 10 6 3 mm (0.4 6 0.1 in.) wide, at least 50 mm (2 in.) long, and0.25 to 0.50 mm (0.01 to 0.02 in.) thicker than the roll clearance to be measured. The lead strips shall be inserted, one at each endof the rolls approximately 25 mm (1 in.
34、) from the guides, while a piece of compounded rubber, with Mooney viscosity in excessof 50 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 portionof the rolls. The rolls shall be at the temperature specified for mixing. After the lead strip
35、s have passed through the rolls, measurethe thickness of the strips to the nearest 0.02 mm (0.001 in.). Tolerance on a roll clearance shall be 610 % or 0.05 mm (0.002 in.),whichever is larger.6.2 Standard Internal MixerThe standard internal mixer shall have a chamber of 1575 6 50 cm3 volume and two
36、rotors withapproximately 400-cm3 displacement volume, resulting in 1170 6 40-cm3 loading capacity. The slow rotor speed shall be 8.16rad/s (77 rpm) and the gear ratio shall be 1:1.125. The rotor wing tip to side clearance shall be 2.4 + 0.3, 0.1 mm(0.094 + 0.010, 0.005 in.). The mixer shall be equip
37、ped with a thermocouple for measuring and recording batch mixingtemperatures. The thermocouple shall be installed through the end frame and shall protrude into the mixing chamber 25 6 2.5 mm(1 6 0.1 in.) measured along the top side of the thermocouple probe. A ram that is 56 6 3 mm by 140 6 8 mm (2.
38、2 6 0.1 in.by 5.5 6 0.3 in.) shall exert a force of 1.27 6 0.06 kN (285 6 14 lbf) on the batch in the chamber. The sides shall be hingedto swing open, made of cast stainless steel and jacketed for controlling temperature by means of a circulating liquid or steam. Theend frames shall be of ductile ir
39、on that has a 0.20 6 0.02-mm (0.008 6 0.001-in.) thick chrome plating on the working surfaces.Rotors are of stainless steel, nitrided, drilled, and equipped with rotary unions for controlling the rotor temperature by means ofa circulating liquid or steam.NOTE 2If internal mixers of other sizes are u
40、sed, adjustments of batch masses and rotor speeds or mixing cycles will be required to obtain equivalentresults.6.3 Standard Miniature Internal Mixer (MIM):6.3.1 The standard miniature internal mixer shall be equipped with a stainless steel mixer head having a bowl of 120-cm3volume and stainless ste
41、el cam-style mixer rotors (removable or fixed) of 34 to 35-cm3 displacement, thus resulting in a 85 61-cm3 volume. The recommended loading is 75 % (64 cm3). The fast or driving rotor (left) shall turn at 6.28 + 3.14 rad/s(60 + 3, 0 rpm) and the gear ratio (drive to driven) shall be 1.5:1. The mixer
42、shall be equipped with a thermocouple installedthrough the ridge in the bowl for measuring and recording the batch temperatures. The mixing chamber shall be closed during themixing cycle by means of a lever or ram. The head and the backplate shall be maintained at the required temperature eitherelec
43、trically or by means of a thermal liquid medium.NOTE 3If miniature internal mixers equipped with Banbury-style mixer head and rotors or heads of other sizes are used, adjustments of batch masses,rotor speeds, or mixing cycles will be required to obtain equivalent results.6.3.2 The miniature internal
44、 mixer may be equipped with a torque-measuring instrument and recorder, which are not essentialfor the mixing operation. If used, it must be calibrated occasionally and after each overhaul of the miniature internal mixer usingthe manufacturers instructions.7. General Mixing Procedures7.1 Mill Mixing
45、 Procedure:7.1.1 Mix compounds with the rubber banded on the slow roll, unless otherwise specified.7.1.2 Measure the temperature of the surfaces of the rolls at a point approximately equidistant from the ends during the mixingoperation either continuously on a recorder or with a manual device having
46、 an accuracy of at least 61C (62F), frequentlyenough to maintain the desired temperature. The batch may be removed momentarily from the mill to measure the surfacetemperature of the slow roll.7.1.3 Whenever 34 cuts are specified, cut the batch 34 of the distance across the roll and hold the knife at
47、 this position until thebank just disappears. Make successive 34 cuts from alternate ends of the roll, allowing 20 s between each cut unless otherwisespecified.7.1.4 Do not cut any batch while free materials are evident in the bank or on the milling surface.7.1.5 Add carbon black evenly across the m
48、ill at a uniform rate. Add all other dry materials slowly and evenly in prescribedtimes. Oil, if required, may be added alternately with carbon black. Carefully collect materials falling through the nip from the trayand return to the mix.7.1.6 Conclude the mixing cycle by passing the rolled batch en
49、dwise 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 setting of 6 mm (.25(0.25 in.), folding it back on itself each time.D3182 15a37.1.8 Weigh the batch and record the mass. If required, cut samples from the batch to allow testing of compound viscosity andprocessability in accordance withTest Methods D1646 orTest Method D6204, and vulcanization characteristics in accordance withTest Methods D2084 or D5289. If tensile st
