1、Designation: D2414 13D2414 13aStandard 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 Department of Defense.1. Scope1.1 This test method covers the determination of the oil ab
3、sorption 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, associated with its use. It is the responsibilityof the use
4、r of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D445 Test Method for Kinematic Viscosity of Transparent and Opaque Liquids (and Calculation of Dynamic Viscosity)D1
5、218 Test Method for Refractive Index and Refractive Dispersion of Hydrocarbon LiquidsD1765 Classification System for Carbon Blacks Used in Rubber ProductsD1799 Practice for Carbon BlackSampling Packaged ShipmentsD1900 Practice for Carbon BlackSampling Bulk ShipmentsD4052 Test Method for Density, Rel
6、ative 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 for Carbon BlackValidation of Test Method Precision and BiasD5554 Test Method for Determination of th
7、e 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 acid value and acidity3. Summary of Test Method3.1 In this test method, oil is added by means of a const
8、ant-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,with an accompanying increase in viscosity. This increased viscosity is transmitted to the torque-sens
9、ing 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 the direct-reading buret. The volume of oil per unit mass of carbon blackis the oil absorption number.
10、3.2 Either DBP, paraffin or epoxidized sunflower oils are acceptable for use with most standard pelleted grades of carbon blackincluding N-series carbon blacks found in Classification D1765. OAN testing using paraffin oils or epoxidized sunflower oils onsome standard blacks and specialty blacks incl
11、uding powder products may result in unacceptable differences as compared to OANtesting with DBP oil. Paraffin and epoxidized sunflower oils are considered non-hazardous; some paraffin oils are FDA approved.For any of the oils, Sections 8 11 (Calibration, Procedure, Calculation, and Report) are to be
12、 consistent with the oil selected foruse. Referee testing between suppliers and users should use DBP oil until such time that precision data are available for alternateoils.1 This test method is under the jurisdiction ofASTM Committee D24 on Carbon Black and is the direct responsibility of Subcommit
13、tee D24.11 on Carbon Black Structure.Current edition approved July 1, 2013Nov. 1, 2013. Published August 2013November 2013. Originally approved in 1965. Last previous edition approved in 20122013as D2414 12.D2414 13. DOI: 10.1520/D2414-13.10.1520/D2414-13A.2 For referencedASTM standards, visit theAS
14、TM 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.3 Available from Deutsches Institut fur Normung e.V.(DIN), Burggrafenstrasse 6, 10787 Berlin, Germany, h
15、ttp:/www.din.de.This document is not an ASTM standard and is intended only 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 c
16、onsult prior editions as appropriate. In all cases only the current versionof 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. Significance and Use4.1 The o
17、il absorption number of a carbon black is related to the processing and vulcanizate properties of rubber compoundscontaining the carbon black.5. Apparatus45.1 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-m
18、m.5.4 Absorptometer, equipped with a constant-rate buret that delivers 4 6 0.024 cm3/min.55.5 Desiccator.6. Reagent and Standards6.1 Purity of ReagentsReagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that allreagents shall conform to the specifications o
19、f the Committee on Analytical Reagents of the American Chemical Society, wheresuch specifications are available.6 Other grades may be used, provided it is first ascertained that the reagent is of sufficiently highpurity to permit its use without lessening the accuracy of the determination.6.2 n-Dibu
20、tyl 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 viscosity 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-P
21、hillips, and LC1 oil from LabChemicals, Germany. All three oils are pharmaceutical or food grade oil, or both, based on available data.6.4 Epoxidized Fatty Acid Ester (EFA), meeting the specifications listed in Annex A4. It is recommended to store the productat temperatures between 7 and 30C. If sto
22、red 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 Standard Reference Blacks, SRB.77. Sampling7.1 Samples shall be taken in accordance with Practices D1799 and D1900.8. Calibration and Standardizatio
23、n8.1 Absorptometer:8.1.1 ModelThree different types of absorptometers are in use: (1) early models based on springs and mechanical indicationof torque (TypeAand B), (2) second generation absorptometers equipped with load cells and digital torque display (Type E8), and(3) current model absorptometers
24、 which are designed with a torque measuring system that includes a micro-computer and softwareto continuously record torque and oil volume with time (Types H and C and modified Type E8). Types A, B, and E8 are designedto stop mixing at a predetermined, fixed torque level, which is the recommended pr
25、ocedure for measuring hard or tread blacks(calibration Procedure A). The computer controlled models (Types H and C and modified Type E8) 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
26、and C and modified Type E8 absorptometers can also provide an end-point at a fixed or 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
27、 the load cell, the torque limit switch or the indicator setpoint, 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 are properly adjusted to achieve ac
28、ceptable 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 referencestandards. The surface finish of
29、 the mixer chamber is critical for maintaining proper calibration, and the bowl should not bemodified to achieve calibration.4 All apparatus are to be operated and maintained in accordance with the manufacturers directions for optimum performance.5 Available from C. W. Brabender Instruments, Inc., 5
30、0 E. Wesley St., Sout Hackensack, NJ 07606 () and from HITEC Luxembourg, 5 Rue de lEglise,L-1458 Luxembourg (www.hitec.lu).6 Reagent Chemicals, American Chemical Society Specifications , American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed bythe American C
31、hemical Society, see Analar 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.7 The sole source of supply of ASTM Standard Reference Blacks known to the committee at th
32、is time is Laboratory Standards 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
33、 which you may attend.8 Type E absorptometers can be modified with additional hardware and micro-computer system.D2414 13a2NOTE 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 m(100 6 15 in.) based upon 8 measureme
34、nts. 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 is recommended that new replacement s
35、tainless steel bowls should also be pre-polished in the same manner (see Annex A3).8.2 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 a gear, one blade spins at 125 r/min, the other
36、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 that the torque spring is adjusted so that the S
37、RB 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 absorptometers Type E, C, and H are calibrated by the man
38、ufacturer 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 calibration should not be confused with the torque limit
39、 switch described in 8.2.5.8.2.4 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. The Type Eabsorptometer has an electronic dampi
40、ng option and Types C and H have appropriate software damping. Make sure that thesedamping options are activated.8.2.5 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 t
41、o be selected using one of the following three procedures:8.2.5.1 Procedure A: End-Point at Fixed Torque LevelThis “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 bla
42、cks. 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 t
43、o setting the TLS based on the SRB F standard; for these absorptometers, set the TLS to 3500mNm for DBP oil, or 4000 mNm for paraffin oil.8.2.5.2 Procedure B: End-Point at 70 % of the Maximum TorqueCertain carcass blacks and thermal blacks may fail to givean end-point due to insufficient torque leve
44、l. Therefore, the preferred method for testing soft blacks is to record the torque curveusing a chart-recorder or a data acquisition system and to read the end-point at 70 % of the maximum of the torque achieved. Setthe TLS or the indicator set point to full scale in order to disable the automatic s
45、hut-off of the absorptometer.8.2.5.3 Procedure C: End-Point at a Fixed, But Reduced Torque LevelRequires use of SRB-5 series standards. See TestMethod D2414 00.8.3 Normalization:8.3.1 Physically calibrate the test apparatus including TLS adjustment using the instructions in 8.2.8.3.2 Test the six AS
46、TM Standard Reference Blacks (SRBs) in duplicate to establish the average measured value. Additionalvalues are added periodically, typically on a weekly basis. The rolling average of the measured values is computed from the latestfour values.NOTE 4When only tread- or carcass-type carbon blacks are t
47、o be tested, the calibration can be limited to either the three tread- (A, B, C) or the threecarcass-type (D, E, F) carbon black standards.8.3.3 Perform a regression analysis using the standard value of the standard (y value) and the rolling average measured value(x value). Separate carcass and trea
48、d calibration curves should be maintained.8.3.4 Normalize the values of all subsequent samples as follows:Normalized value5measured value3slope!1y 2intercept (1)8.3.5 For normalized values of the SRBs that are consistently outside the x-chart limits listed in Guide D4821, the test apparatusshould be
49、 recalibrated in accordance with 8.2.8.3.6 When any absorptometer or calibration changes occur, a new calibration curve must be initiated as described in 8.3.2.8.3.7 In most instances, if proper calibration cannot be achieved by following 8.2 or 8.3.2 8.3.4, it will be necessary to replacethe mixer chamber with one of proper surface finish. Review Appendix X1.9. Procedure9.1 Dry an adequate sample for 1 h in the specified oven set at 125C. Prior to testing, cool the sample in a desiccator for amini
