1、Designation: D2414 161D2414 17Standard Test Method forCarbon BlackOil Absorption Number (OAN)1This standard is issued under the fixed designation D2414; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A n
2、umber 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 Defense.1 NOTECorrected 5.4 editorially in October 2016.1. Scope1.1 Th
3、is test method covers the determination of the oil absorption number of carbon black.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, associ
4、ated with its use. It is the responsibilityof the user of this standard to establish appropriate safety safety, health, and healthenvironmental practices and determine theapplicability of regulatory limitations prior to use.1.4 This international standard was developed in accordance with internation
5、ally recognized principles on standardizationestablished in the Decision on Principles for the Development of International Standards, Guides and Recommendations issuedby the World Trade Organization Technical Barriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D445 Test Met
6、hod for Kinematic Viscosity of Transparent and Opaque Liquids (and Calculation of Dynamic Viscosity)D1218 Test Method for Refractive Index and Refractive Dispersion of Hydrocarbon LiquidsD1765 Classification System for Carbon Blacks Used in Rubber ProductsD1799 Practice for Carbon BlackSampling Pack
7、aged ShipmentsD1900 Practice for Carbon BlackSampling Bulk ShipmentsD4052 Test Method for Density, Relative Density, and API Gravity of Liquids by Digital Density MeterD4483 Practice for Evaluating Precision for Test Method Standards in the Rubber and Carbon Black Manufacturing IndustriesD4821 Guide
8、 for Carbon BlackValidation of Test Method Precision and BiasD5554 Test Method for Determination of the Iodine Value of Fats and Oils2.2 DIN Standards:3DIN 16945 Testing of resins, hardeners and accelerators, and catalyzed resinsDIN EN ISO 660 Animal and vegetable fats and oils - Determination of ac
9、id value and acidity3. Summary of Test Method3.1 In this test method, oil is added by means of a constant-rate buret to a sample of carbon black in the mixer chamber of anabsorptometer.As the sample absorbs the oil, the mixture changes from a free-flowing state to one of a semiplastic agglomeration,
10、with an accompanying increase in viscosity. This increased viscosity is transmitted to the torque-sensing system of theabsorptometer. When the viscosity of the mixture reaches a predetermined torque level, the absorptometer and buret will shut offsimultaneously. The volume of oil added is read from
11、the direct-reading buret. The volume of oil per unit mass of carbon blackis the oil absorption number.3.2 Either DBP, paraffin or epoxidized sunflower Epoxidized Fatty Acid Ester (EFA) oils are acceptable for use with moststandard pelleted grades of carbon black including N-series carbon blacks foun
12、d in Classification D1765. OAN testing using1 This test method is under the jurisdiction ofASTM Committee D24 on Carbon Black and is the direct responsibility of Subcommittee D24.11 on Carbon Black Structure.Current edition approved Jan. 1, 2016Dec. 1, 2017. Published January 2016January 2018. Origi
13、nally approved in 1965. Last previous edition approved in 20142016 asD2414 14.D2414 161. DOI: 10.1520/D2414-16E01.10.1520/D2414-17.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume informat
14、ion, refer to the standards Document Summary page on the ASTM website.3 Available from Deutsches Institut fur Normung e.V.(DIN), Burggrafenstrasse 6, 10787 Berlin, Germany, http:/www.din.de.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indicati
15、on 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 versionof the standard as published by ASTM is to be consi
16、dered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1paraffin oils or epoxidized sunflower EFAoils on some standard blacks and specialty blacks including powder products may resultin unacceptable differences as
17、compared to OAN testing with DBP oil. Paraffin and epoxidized sunflower EFA oils are considerednon-hazardous; some paraffin oils are FDA approved. For any of the oils, Sections 8 1112 (Calibration, Procedure, Calculation,and Report) are to be consistent with the oil selected for use. Referee testing
18、 between suppliers and users should use DBP oil untilsuch time that precision data are available for alternate oils.4. Significance and Use4.1 The oil absorption number of a carbon black is related to the processing and vulcanizate properties of rubber compoundscontaining the carbon black.5. Apparat
19、us45.1 Balance, analytical, with an 0.01-g sensitivity.5.2 Oven, gravity-convection type, capable of maintaining 125 6 5C.5.3 Spatula, rubber, 100-mm.5.4 Absorptometer, equipped with a constant-rate buret that delivers 4 6 0.024 cm3/min.5.5 Desiccator.6. Reagent and Standards6.1 Purity of ReagentsRe
20、agent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that allreagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, wheresuch specifications are available.5 Other grades may be used, provided it i
21、s first ascertained that the reagent is of sufficiently highpurity to permit its use without lessening the accuracy of the determination.6.2 n-Dibutyl Phthalate, having a density of 1.042 to 1.047 Mg/m3 at 25C and a relative density of 1.045 to 1.050 at 25C.6.3 Paraffn Oil, having a kinematic viscos
22、ity of 10 to 34 mm2/s (cSt) at 40C.NOTE 1Three paraffin oils have been found suitable including Marcol 82 from Exxon, 80/90 White Oil from Conoco-Phillips, and LC1 oil from LabChemicals, Germany. All three oils are pharmaceutical or food grade oil, or both, based on available data.6.4 Epoxidized Fat
23、ty Acid Ester (EFA), meeting the specifications listed in Annex A4. It is recommended to store the productat temperatures between 7 and 30C. If stored in sealed original containers, the product is stable for at least 12 months. Forhandling and safety, please refer to safety data sheet.6.5 ASTM D24 S
24、tandard Reference Blacks, SRB.67. Sampling7.1 Samples shall be taken in accordance with Practices D1799 and D1900.8. Calibration and StandardizationOil Absorptometers, Instrument Calibration, and End-Point Procedures8.1 Absorptometer:8.1.1 ModelThree different types of absorptometers are in use: (1)
25、 early models based on springs and mechanical indicationof torque (TypeAand B), (2) second generation absorptometers equipped with load cells and digital torque display (Type E7), and(3) current model absorptometers which are designed with a torque measuring system that includes a micro-computer and
26、 softwareto continuously record torque and oil volume with time (Types H and C and modified Type E7). Types A, B, and E7 are designedto stop mixing at a predetermined, fixed torque level, which is the recommended procedure for measuring hard or tread blacks(calibration Procedure A). The computer con
27、trolled models (Types H and C and modified Type E7) are required for runningcalibration Procedure B, the recommended torque curve analysis for the determination of the end-point of soft or carcass blacks.The Type H and C and modified Type E7 absorptometers can also provide an end-point at a fixed or
28、 predetermined torque levelsuch that these types of absorptometers are well-suited for measuring OAN of both hard and soft carbon blacks. Severalcomponents influence the calibration: the dynamometer torque spring or the load cell, the torque limit switch or the indicator set4 All apparatus are to be
29、 operated and maintained in accordance with the manufacturers directions for optimum performance.5 Reagent Chemicals, American Chemical Society Specifications , American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed bythe American Chemical Society, see Anala
30、r Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K. and the United States Pharmacopeia and NationalFormulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.6 The sole source of supply of ASTM Standard Reference Blacks known to the committee at this time is Laboratory Stan
31、dards and Technologies, 227 Somerset, Borger,TX 79007, http:/ If you are aware of alternative suppliers, please provide this information to ASTM International Headquarters. Your comments willreceive careful consideration at a meeting of the responsible technical committee,1 which you may attend.7 Ty
32、pe E absorptometers can be modified with additional hardware and micro-computer system.D2414 172point, the damper (oil damper or electronic damping), and the mixing head consisting of two counter rotating blades and a mixingbowl. It is necessary that all of these components are in good condition and
33、 are properly adjusted to achieve acceptable calibration.8.1.2 Mixing BowlTypically the absorptometer is delivered with either a surface-treated stainless steel or anodized aluminummixing bowl. These bowls are considered acceptable provided they give the correct reading for the appropriate SRB refer
34、encestandards. The surface finish of the mixer chamber is critical for maintaining proper calibration, and the bowl should not bemodified to achieve calibration.NOTE 2Stainless steel chambers have been found satisfactory for the test when they are manufactured to a roughness value (Ra) of 2.5 6 0.4
35、m(100 6 15 in.) based upon 8 measurements. No single measurement should be greater than 3.6 m (140 in.) or less than 1.5 m (60 in.). Stainlesssteel bowls purchased with an absorptometer have been pre-polished for 16 h to minimize bowl surface changes affecting calibration during their initialuse. It
36、 is recommended that new replacement stainless steel bowls should also be pre-polished in the same manner (see Annex A3).8.2 Instrument Calibration:8.2.1 Rotor BladesThe speed of the motor driving the rotor blades is either fixed (Type A and B) or has to be set (Type E,C, and H) to 125 r/min. Due to
37、 a gear, one blade spins at 125 r/min, the other blade at 250 r/min.8.2.2 Constant-Rate BuretThe delivery rate of the buret is to be 4 cm3/min. See Annex A1 for detailed instructions on theprocedure for calibration check of the constant-rate buret.8.2.3 Spring Tension (Type A and B)It is recommended
38、 that the torque spring is adjusted so that the SRB F standard willdevelop a maximum torque between 70 % and full-scale deflection. This is achieved by selecting the appropriate spring strengthand adjusting the spring tension in accordance with the instructions of the manufacturer.NOTE 3The absorpto
39、meters Type E, C, and H are calibrated by the manufacturer to give a direct reading of torque in mNm; this calibration shouldnot be modified in order to achieve a desired level of torque. If calibration is necessary, refer to the instrument manufacturers recommendations. Theinstrument torque calibra
40、tion should not be confused with the torque limit switch described in 8.3.1.8.2.4 DamperFor the Type A absorptometer, it is recommended to keep the valve of the oil damper fully closed. The TypeB absorptometer shall provide a full-scale recovery of 3 6 0.5 s; the valve has to be adjusted accordingly
41、. The Type Eabsorptometer has an electronic damping option and Types C and H have appropriate software damping. Make sure that thesedamping options are activated.8.2.5 Stainless Mixing BowlsWhen replacing an old mixing bowl with a new one, further pre-polish may be needed afterinstallation even if t
42、hose mixing bowls are typically already pre-polished by the manufacturer. The surface finish of the mixerchamber is critical for maintaining proper calibration, and the bowl shall not be modified to achieve calibration other than describedin Annex A3.8.3 Calibration: End-Point Procedures:8.2.1 Rotor
43、 BladesThe speed of the motor driving the rotor blades is either fixed (Type A and B) or has to be set (Type E,C, and H) to 125 r/min. Due to a gear, one blade spins at 125 r/min, the other blade at 250 r/min.8.2.2 Constant-Rate BuretThe delivery rate of the buret is to be 4 cm3/min. See Annex A1 fo
44、r detailed instructions on theprocedure for calibration check of the constant-rate buret.8.2.3 Spring Tension (Type A and B)It is recommended that the torque spring is adjusted so that the SRB F standard willdevelop a maximum torque between 70 % and full-scale deflection. This is achieved by selecti
45、ng the appropriate spring strengthand adjusting the spring tension in accordance with the instructions of the manufacturer.NOTE 3The absorptometers Type E, C, and H are calibrated by the manufacturer to give a direct reading of torque in mNm; this calibration shouldnot be modified in order to achiev
46、e a desired level of torque. If calibration is necessary, refer to the instrument manufacturers recommendations. Theinstrument torque calibration should not be confused with the torque limit switch described in 8.2.5.8.2.4 DamperFor the Type A absorptometer, it is recommended to keep the valve of th
47、e oil damper fully closed. The TypeB absorptometer shall provide a full-scale recovery of 3 6 0.5 s; the valve has to be adjusted accordingly. The Type Eabsorptometer has an electronic damping option and Types C and H have appropriate software damping. Make sure that thesedamping options are activat
48、ed.8.3.1 Torque Limit Switch (TLS) or the Indicator Set PointIf the end-point of the test is determined by a fixed torque limit,the setting of the TLS, also called indicator set-point, has to be selected using one of the following three procedures:8.3.1.1 Procedure A: End-Point at Fixed Torque Level
49、This “classical” method is well suited for most hard or tread blacks butmay lead to problems when low-torque carcass blacks are to be tested; proceed to Procedure B for low-torque carbon blacks. ForType A, B, and E absorptometers, adjust the TLS or the indicator set point in such way that the current SRB F standard gives thecorrect target value within the limits as defined in Guide D4821. For Type E, C, and H absorptometers dedicated to testing treadblacks only, there is no advantage to setting the TLS based on th
