1、Designation: D2414 13Standard 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 number in
2、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 oilabsorption n
3、umber of carbon black.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 sta
4、ndard 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:2D445 Test Method for Kinematic Viscosity of Transparentand Opaque Liquids (and Calculation of Dynamic Viscos-ity)D1218 Test M
5、ethod for Refractive Index and RefractiveDispersion of Hydrocarbon LiquidsD1765 Classification System for Carbon Blacks Used inRubber ProductsD1799 Practice for Carbon BlackSampling PackagedShipmentsD1900 Practice for Carbon BlackSampling Bulk Ship-mentsD4052 Test Method for Density, Relative Densit
6、y, and APIGravity of Liquids by Digital Density MeterD4483 Practice for Evaluating Precision for Test MethodStandards in the Rubber and Carbon Black ManufacturingIndustriesD4821 Guide for Carbon BlackValidation of Test MethodPrecision and BiasD5554 Test Method for Determination of the Iodine Value o
7、fFats and Oils2.2 DIN Standards:3DIN 16945 Testing of resins, hardeners and accelerators, andcatalyzed 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 aconstant-rate buret to a
8、sample of carbon black in the mixerchamber of an absorptometer. As the sample absorbs the oil,the mixture changes from a free-flowing state to one of asemiplastic agglomeration, with an accompanying increase inviscosity. This increased viscosity is transmitted to the torque-sensing system of the abs
9、orptometer. When the viscosity of themixture reaches a predetermined torque level, the absorptom-eter and buret will shut off simultaneously. The volume of oiladded is read from the direct-reading buret. The volume of oilper unit mass of carbon black is the oil absorption number.3.2 Either DBP, para
10、ffin or epoxidized sunflower oils areacceptable for use with most standard pelleted grades of carbonblack including N-series carbon blacks found in ClassificationD1765. OAN testing using paraffin oils or epoxidized sun-flower oils on some standard blacks and specialty blacksincluding powder products
11、 may result in unacceptable differ-ences as compared to OAN testing with DBP oil. Paraffin andepoxidized sunflower oils are considered non-hazardous; someparaffin oils are FDA approved. For any of the oils, Sections8-11 (Calibration, Procedure, Calculation, and Report) are tobe consistent with the o
12、il selected for use. Referee testingbetween suppliers and users should use DBPoil until such timethat precision data are available for alternate oils.4. Significance and Use4.1 The oil absorption number of a carbon black is related tothe processing and vulcanizate properties of rubber compoundsconta
13、ining the carbon black.1This test method is under the jurisdiction ofASTM Committee D24 on CarbonBlack and is the direct responsibility of Subcommittee D24.11 on Carbon BlackStructure.Current edition approved July 1, 2013. Published August 2013. Originallyapproved in 1965. Last previous edition appr
14、oved in 2012 as D2414 12. DOI:10.1520/D2414-13.2For 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.3Available fro
15、m Deutsches Institut fur Normung e.V.(DIN), Burggrafenstrasse 6,10787 Berlin, Germany, http:/www.din.de.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States15. Apparatus45.1 Balance, analytical, with an 0.01-g sensitivity.5.2 Oven, gravity
16、-convection type, capable of maintaining125 6 5C.5.3 Spatula, rubber, 100-mm.5.4 Absorptometer, equipped with a constant-rate buret thatdelivers 4 6 0.024 cm3/min.55.5 Desiccator.6. Reagent and Standards6.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicat
17、ed, it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.6Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permi
18、t its use without lessening theaccuracy of the determination.6.2 n-Dibutyl Phthalate, having a density of 1.042 to 1.047Mg/m3at 25C and a relative density of 1.045 to 1.050 at 25C.6.3 Paraffn Oil, having a kinematic viscosity of 10 to34 mm2/s (cSt) at 40C.NOTE 1Three paraffin oils have been found su
19、itable including Marcol82 from Exxon, 80/90 White Oil from Conoco-Phillips, and LC1 oil fromLab Chemicals, Germany. All three oils are pharmaceutical or food gradeoil, or both, based on available data.6.4 Epoxidized Fatty Acid Ester (EFA), meeting the speci-fications listed in Annex A4. It is recomm
20、ended to store theproduct at temperatures between 7 and 30C. If stored in sealedoriginal containers, the product is stable for at least 12 months.For handling and safety, please refer to safety data sheet.6.5 ASTM D24 Standard Reference Blacks, SRB.77. Sampling7.1 Samples shall be taken in accordanc
21、e with PracticesD1799 and D1900.8. Calibration and Standardization8.1 Absorptometer:8.1.1 ModelThree different types of absorptometers are inuse: (1) early models based on springs and mechanical indica-tion of torque (Type A and B), (2) second generation absorp-tometers equipped with load cells and
22、digital torque display(Type E8), and (3) current model absorptometers which aredesigned with a torque measuring system that includes amicro-computer and software to continuously record torqueand oil volume with time (Types H and C and modified TypeE8). Types A, B, and E8are designed to stop mixing a
23、t apredetermined, fixed torque level, which is the recommendedprocedure for measuring hard or tread blacks (calibrationProcedureA). The computer controlled models (Types H and Cand modified Type E8) are required for running calibrationProcedure B, the recommended torque curve analysis for thedetermi
24、nation of the end-point of soft or carcass blacks. TheType H and C and modified Type E8absorptometers can alsoprovide an end-point at a fixed or predetermined torque levelsuch that these types of absorptometers are well-suited formeasuring OAN of both hard and soft carbon blacks. Severalcomponents i
25、nfluence the calibration: the dynamometer torquespring or the load cell, the torque limit switch or the indicatorset point, the damper (oil damper or electronic damping), andthe mixing head consisting of two counter rotating blades anda mixing bowl. It is necessary that all of these components arein
26、 good condition and are properly adjusted to achieve accept-able calibration.8.1.2 Mixing BowlTypically the absorptometer is deliv-ered with either a surface-treated stainless steel or anodizedaluminum mixing bowl. These bowls are considered accept-able provided they give the correct reading for the
27、 appropriateSRB reference standards. The surface finish of the mixerchamber is critical for maintaining proper calibration, and thebowl should not be modified to achieve calibration.NOTE 2Stainless steel chambers have been found satisfactory for thetest when they are manufactured to a roughness valu
28、e (Ra) of 2.5 60.4 m (100 6 15 in.) based upon 8 measurements. No single measure-ment should be greater than 3.6 m (140 in.) or less than 1.5 m (60in.). Stainless steel bowls purchased with an absorptometer have beenpre-polished for 16 h to minimize bowl surface changes affectingcalibration during t
29、heir initial use. It is recommended that new replace-ment stainless 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 therotor blades is either fixed (Type A and B) or has to be set(Type E, C, and H) to 125 r/min
30、. Due to a gear, one blade spinsat 125 r/min, the other blade at 250 r/min.8.2.2 Constant-Rate BuretThe delivery rate of the buret isto be 4 cm3/min. See AnnexA1 for detailed instructions on theprocedure for calibration check of the constant-rate buret.8.2.3 Spring Tension (Type A and B)It is recomm
31、endedthat the torque spring is adjusted so that the SRB F standardwill develop a maximum torque between 70 % and full-scaledeflection. This is achieved by selecting the appropriate springstrength and adjusting the spring tension in accordance with theinstructions of the manufacturer.4All apparatus a
32、re to be operated and maintained in accordance with themanufacturers directions for optimum performance.5Available from C. W. Brabender Instruments, Inc., 50 E. Wesley St., SoutHackensack, NJ 07606 () and from HITEC Luxembourg, 5 Ruede lEglise, L-1458 Luxembourg (www.hitec.lu).6Reagent Chemicals, Am
33、erican Chemical Society Specifications , AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K. and the United States Pharmacopeia andNational Formula
34、ry, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.7The sole source of supply of ASTM Standard Reference Blacks known to thecommittee at this time is Laboratory Standards and Technologies, 227 Somerset,Borger, TX 79007, http:/ If you are aware of alternativesuppliers, please provide this
35、information to ASTM International Headquarters.Your comments will receive careful consideration at a meeting of the responsibletechnical committee,1which you may attend.8Type E absorptometers can be modified with additional hardware and micro-computer system.D2414 132NOTE 3The absorptometers Type E,
36、 C, and H are calibrated by themanufacturer to give a direct reading of torque in mNm; this calibrationshould not be modified in order to achieve a desired level of torque. Ifcalibration is necessary, refer to the instrument manufacturers recommen-dations. The instrument torque calibration should no
37、t be confused with thetorque limit switch described in 8.2.5.8.2.4 DamperFor the Type A absorptometer, it is recom-mended to keep the valve of the oil damper fully closed. TheType B absorptometer shall provide a full-scale recovery of 36 0.5 s; the valve has to be adjusted accordingly. The Type Eabs
38、orptometer has an electronic damping option and Types Cand H have appropriate software damping. Make sure thatthese damping options are activated.8.2.5 Torque Limit Switch (TLS) or the Indicator SetPointIf the end-point of the test is determined by a fixedtorque limit, the setting of the TLS, also c
39、alled indicatorset-point, has to be selected using one of the following threeprocedures:8.2.5.1 Procedure A: End-Point at Fixed Torque LevelThis “classical” method is well suited for most hard or treadblacks but may lead to problems when low-torque carcassblacks are to be tested; proceed to Procedur
40、e B for low-torquecarbon blacks. For TypeA, B, and E absorptometers, adjust theTLS or the indicator set point in such way that the current SRBF standard gives the correct target value within the limits asdefined in Guide D4821. For Type E, C, and H absorptometersdedicated to testing tread blacks onl
41、y, there is no advantage tosetting the TLS based on the SRB F standard; for theseabsorptometers, set theTLS to 3500 mNm for DBPoil, or 4000mNm for paraffin oil.8.2.5.2 Procedure B: End-Point at 70 % of the MaximumTorqueCertain carcass blacks and thermal blacks may fail togive an end-point due to ins
42、ufficient torque level. Therefore,the preferred method for testing soft blacks is to record thetorque curve using a chart-recorder or a data acquisition systemand to read the end-point at 70 % of the maximum of the torqueachieved. Set the TLS or the indicator set point to full scale inorder to disab
43、le the automatic shut-off of the absorptometer.8.2.5.3 Procedure C: End-Point at a Fixed, But ReducedTorque LevelRequires use of SRB-5 series standards. SeeTest Method D2414 00.8.3 Normalization:8.3.1 Physically calibrate the test apparatus including TLSadjustment using the instructions in 8.2.8.3.2
44、 Test the sixASTM Standard Reference Blacks (SRBs)in duplicate to establish the average measured value. Addi-tional values are added periodically, typically on a weeklybasis. The rolling average of the measured values is computedfrom the latest four values.NOTE 4When only tread- or carcass-type carb
45、on blacks are to betested, the calibration can be limited to either the three tread- (A, B, C) orthe three carcass-type (D, E, F) carbon black standards.8.3.3 Perform a regression analysis using the standard valueof the standard (y value) and the rolling average measuredvalue (x value). Separate car
46、cass and tread calibration curvesshould be maintained.8.3.4 Normalize the values of all subsequent samples asfollows:Normalized value 5 measured value 3slope!1y 2 intercept (1)8.3.5 For normalized values of the SRBs that are consis-tently outside the x-chart limits listed in Guide D4821, the testapp
47、aratus should be 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 beachieved by following 8.2 or 8.3.2-8.3.4, it will be necessary torepl
48、ace the mixer chamber with one of proper surface finish.9. Procedure9.1 Dry an adequate sample for1hinthespecified oven setat 125C. Prior to testing, cool the sample in a desiccator for aminimum of 30 min.9.2 Weigh the sample to the nearest 0.01 g. The recom-mended masses are as follows:Carbon Black
49、 Mass, gN630, N642, and N700 series, except N765 25N800 and N900 series, SRB D-7 and D-8 40All others 209.3 It is recommended that a testing temperature of 23 65C be maintained, as measured by a thermocouple in themixing bowl. If a temperature controllable mixing bowl is notavailable, keep the bowl temperature below 30C and complywith Note 5 and Note 6 while running the samples.NOTE 5If the absorptometer has remained idle for more than 15 minand a temperature controllable bowl is not being used, a 10-mi
