ASTM D3493-2018 Standard Test Method for Carbon Black&x2014 Oil Absorption Number of Compressed Sample (COAN).pdf

1、Designation: D3493 18Standard Test Method forCarbon BlackOil Absorption Number of CompressedSample (COAN)1This standard is issued under the fixed designation D3493; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last r

2、evision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the procedure for the mechani-cal compression of a carbon black sample and the determina-tion of the

3、 oil absorption number of the compressed sample.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 theresponsibili

4、ty of the user of this standard to establish appro-priate safety, health, and environmental practices and deter-mine the applicability of regulatory limitations prior to use.1.4 This international standard was developed in accor-dance with internationally recognized principles on standard-ization es

5、tablished in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D1765 Classification System for Carbon Blacks Used inRubber

6、ProductsD1799 Practice for Carbon BlackSampling PackagedShipmentsD1900 Practice for Carbon BlackSampling Bulk Ship-mentsD2414 Test Method for Carbon BlackOil AbsorptionNumber (OAN)D4821 Guide for Carbon BlackValidation of Test MethodPrecision and BiasD4483 Practice for Evaluating Precision for Test

7、MethodStandards in the Rubber and Carbon Black ManufacturingIndustries3. Summary of Test Method3.1 A sample of carbon black is compressed four times in acompression cylinder at a pressure of 165 MPa (24 000 psi)and then tested in an absorptometer to determine the oilabsorption number.3.2 n-Dibutyl p

8、hthalate, paraffin oil, or EFA oil is added bymeans of a constant-rate buret to the compressed sample ofcarbon black in the mixer chamber of an absorptometer.As thesample absorbs the oil, the mixture changes from a free-flowing state to one of a semiplastic agglomeration, with anaccompanying increas

9、e in viscosity. This increased viscosity istransmitted to the torque-sensing system of the absorptometer.When the viscosity of the mixture reaches a predeterminedtorque level, the absorptometer and buret will simultaneouslyshut off. The volume of oil added is read from the directreading buret. The v

10、olume of oil per unit mass of carbon blackis the oil absorption number. Either DBP, paraffin oil, or EFAoil is acceptable for use with many standard pelleted grades ofN-series carbon blacks found in Classification D1765. COANtesting using paraffin oil or EFA oil on some specialty blacksand powder bl

11、acks may result in significant differences whencompared to COAN testing using DBP oil. Referee testingbetween suppliers and users should use DBPoil until such timethat precision data is available for paraffin and EFA oils.4. Significance and Use4.1 The oil absorption number of a carbon black is rela

12、ted tothe processing and vulcanizate properties of rubber compoundscontaining the carbon black.4.2 The difference between the regular oil absorption num-ber and the oil absorption number of compressed sample issome measure of the stability of the structure of the carbonblack.5. Apparatus35.1 Balance

13、, analytical, 0.01-g sensitivity.1This test method is under the jurisdiction of ASTM Committee D24 on CarbonBlack and is the direct responsibility of Subcommittee D24.11 on Carbon BlackStructure.Current edition approved July 1, 2018. Published August 2018. Originallyapproved in 1976. Last previous e

14、dition approved in 2016 as D3493 16. DOI:10.1520/D3493-18.2For 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.3Ea

15、ch apparatus is to be operated and maintained in accordance with themanufacturers directions for optimum performance.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internati

16、onally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.15.2 Oven, gravity-convection type, capable of mainta

17、ining125C 6 5C.5.3 Carbon Black Press, capable of compressing a 25-gsample to 165 MPa (24 000 psi).5.4 Absorptometer, equipped with a constant-rate buret thatdelivers 67 6 0.4 mm3/s (4 6 0.024 cm3/min).5.5 Spatula, rubber, 100 mm.5.6 Sieve, 850 m (U.S. No. 20), approximately 125-mm(5-in.) diameter w

18、ith receiver pan.5.7 Brush, approximately 40 mm (1.5 in.), stiff bristle.5.8 Desiccator.6. Reagent and Standards6.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the specifications of the Commit-tee o

19、n Analytical Reagents of the American Chemical Society,where such specifications are available.4Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.6.2 n-Dibutyl Phthalate, havin

20、g a density of 1.042 to1.047 mgm3at 25C and a relative density of 1.045 to 1.050at 25C.6.3 Paraffn Oil, having a kinematic viscosity of 10 to34 mm2/s (cSt) at 40C.56.4 Epoxidized Fatty Acid Ester (EFA), meeting the speci-fications listed in Test Method D2414, Table 1. It is recom-mended to store the

21、 product at temperatures between 7 and30C. If stored in sealed original containers, the product isstable for at least 12 months. For handling and safety, pleaserefer to safety data sheet.6.5 ASTM D24 Standard Reference Blacks, SRB.67. Sampling7.1 Samples shall be taken in accordance with PracticesD1

22、799 and D1900.8. Calibration and Standardization8.1 See Test Method D2414.NOTE 1If values are not obtained within the acceptable range, it willbe necessary to either vary the pressure of the hydraulic press untilacceptable values are obtained or follow Guide D4821.9. Procedure9.1 Dry an adequate sam

23、ple for1hinaspecified oven setat 125C. Cool the sample in a desiccator for a minimum of30 min prior to testing.9.2 Weigh a sample mass of either 25, 30, or 45 g dependingon the sample mass requirement for oil absorption per TestMethod D2414. The desired sample mass to be compressedwill weigh 5 6 0.1

24、 g greater than the mass specified insubsection 9.2 of Test Method D2414.9.3 Compress the sample using a carbon black press per themanufacturer instructions.9.4 A general procedure for compressing carbon blackinvolves the following steps:9.4.1 Ensure the cylinder and piston tips are clean.9.4.2 Open

25、 the press by moving the pistons is a properposition to add carbon black.9.4.3 Add the desired amount of carbon black to thecylinder using a funnel.9.4.4 Compress the carbon black to approximately 165 MPa(24 000 psi), hold for about 1 s, then release.9.4.5 Open the press to release the carbon black

26、in thefunnel.9.4.6 Break up the carbon black using a spatula.9.4.7 Return the sample to the cylinder.9.4.8 Repeat 9.4.4 9.4.7 three additional times for a totalof four compressions.9.4.9 Open the press to release the sample from the cylinder.9.4.10 Transfer the compressed carbon black to a clean850-

27、m sieve (sieve #20); break up the sample using a spatulaand pass it through the sieve.9.4.11 Retain the sample from 9.4.10 for testing. Proceed to9.5.NOTE 2If the compressed sample is not to be tested within 15 minafter compression, it should be stored in a desiccator or dried for1hinthespecified ov

28、en set at 125C prior to testing.9.5 Measure the oil absorption number of the compressedsample in accordance with Test Method D2414. Use the samesample masses as recommended in subsection 9.2 of TestMethod D2414.10. Calculation10.1 Calculate the oil absorption number, compressedsample, to the nearest

29、 0.1 105m3/kg (cm3/100 g) as follows:Oil absorption number, compressed sample, 1025m3/kg5AB3100where:A = volume of oil used, cm3, andB = mass of tested sample, g.4Reagent Chemicals, American Chemical Society Specifications , AmericanChemical Society, Washington, DC. For suggestions on the testing of

30、 reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.5The sole source of supply of paraffin oil (Marcol 82,

31、 which has beendemonstrated to provide comparable results to DBP oil) known to the committee atthis time is Exxon. If you are aware of alternative suppliers, please provide thisinformation to ASTM International Headquarters. Your comments will receivecareful consideration at a meeting of the respons

32、ible technical committee,1whichyou may attend.6The sole source of supply of theASTM 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 information t

33、o ASTM International Headquarters.Your comments will receive careful consideration at a meeting of the responsibletechnical committee,1which you may attend.D3493 18211. Report11.1 Report the following information:11.1.1 Proper identification of the sample,11.1.2 The result obtained from the individu

34、al determina-tion is reported to the nearest 0.1 105m3/kg (cm3/100 g),11.1.3 Results obtained with DBP, paraffin oil or EFA oil,and11.1.4 Method for end-point determination (ProcedureA, B,or C on Standardization in Test Method D2414).12. Precision and Bias12.1 These precision statements have been pr

35、epared inaccordance with Practice D4483. Refer to this practice forterminology and other statistical details.12.2 Interlaboratory precision program (ITP) informationwas conducted as detailed in Table 1. Both repeatability andreproducibility represent short-term (daily) testing conditions.The testing

36、 was performed using two operators in eachlaboratory performing the test once on each of two days (totalof four tests). A test result is the value obtained from a singledetermination. Acceptable difference values were not mea-sured. The between operator component of variation is in-cluded in the cal

37、culated values for r and R.12.3 The precision results in this precision and bias sectiongive an estimate of the precision of this test method with thematerials used in the particular interlaboratory programs de-scribed in 12.2. The precision parameters should not be usedfor acceptance or rejection t

38、esting of any group of materialswithout documentation that they are applicable to those par-ticular materials and the specific testing protocols of the testmethod. Any appropriate value may be used from Table 2.12.4 The results of the precision calculations for this test aregiven in Table 2. The mat

39、erials are arranged in ascending“mean level” order.12.5 RepeatabilityThe pooled relative repeatability, (r),of this test has been established as 1.4 %. Any other value inTable 2 may be used as an estimate of repeatability, asappropriate. The difference between two single test results (ordeterminatio

40、ns) found on identical test material under therepeatability conditions prescribed for this test will exceed therepeatability on an average of not more than once in 20 casesin the normal and correct operation of the method. Two singletest results that differ by more than the appropriate value fromTab

41、le 2 must be suspected of being from different populationsand some appropriate action taken.NOTE 3Appropriate action may be an investigation of the test methodprocedure or apparatus for faulty operation or the declaration of asignificant difference in the two materials, samples, and so forth, whichg

42、enerated the two test results.12.6 ReproducibilityThe pooled relative reproducibility,(R), of this test method has been established as 3.6 %. Anyother value in Table 2 may be used as an estimate ofreproducibility, as appropriate. The difference between twosingle and independent test results found by

43、 two operatorsworking under the prescribed reproducibility conditions indifferent laboratories on identical test material will exceed thereproducibility on an average of not more than once in 20 casesin the normal and correct operation of the method. Two singletest results produced in different labo

44、ratories that differ bymore than the appropriate value from Table 2 must besuspected of being from different populations and some appro-priate investigative or technical/commercial action taken.12.7 BiasIn test method terminology, bias is the differencebetween an average test value and the reference

45、 (true) testproperty value. Reference values do not exist for this testTABLE 1 SRB8 ITP InformationNumber of Labs (M/H/L)SRB8 Material Grade Producer Test Period D3493SRB-8A N326 Continental March 2008 64 (1/0/0)SRB-8A2 N326 Continental March 2013 72 (0/1/1)SRB-8B N134 Cabot June 2009 66 (0/0/0)SRB-

46、8B2 N134 Cabot March/April 2014 40 (3/4/3)SRB-8C HS Tread Columbian September 2010 66 (2/1/0)SRB-8D LS Carcass Cabot March 2009 67 (0/2/0)SRB-8E N660 Orion September 2008 57 (1/0/0)SRB-8F N683 Orion March 2010 67 (1/1/0)SRB-8F2 N683 Orion March 2015 62 (1/0/0)SRB-8GAN990 Cancarb Last half of 1996 Un

47、knownASRB-8G was produced and approved in the last half of 1996 as SRB-5G and has continued to be included in the current SRB sets since that time. At the time it wasproduced and approved it was D24s practice to only publish the within-laboratory standard deviation, Sr, and associated limits. The be

48、tween-laboratory standard deviation,SR, was never published and since the data is no longer available it is not possible to calculate or publish the SR values and corresponding limits. The SRB G materialwas only tested for NSA, STSA, and OAN per the test method version available in 1996.TABLE 2 Prec

49、ision Parameters for Test Method D3493, COANMethod (Type 1 Precision)AUnits105m3/kg(cm3/100 g)MaterialMeanLevelSr r (r) SR R (R)SRB-8C 130.6 0.54 1.52 1.2 1.47 4.17 3.2SRB-8B2 103.1 0.50 1.42 1.4 1.03 2.92 2.8SRB-8B 99.4 0.47 1.32 1.3 1.03 2.91 2.9SRB-8A2 67.5 0.35 0.98 1.5 1.08 3.05 4.5SRB-8A 66.7 0.42 1.20 1.8 0.87 2.46 3.7SRB-8F 88.6 0.40 1.12 1.3 0.91 2.58 2.9SRB-8E 74.7 0.36 1.01 1.3 0.99 2.82 3.8SRB-8D 36.9 0.26 0.74 1.9 0.96 2.72 7.1Average 83.7Pooled Values 0.42 1.19 1.4 1.06 2.99 3.6AThe preferred precision values are