1、Designation: D3493 18aStandard 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
2、revision. 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 th
3、e 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 theresponsibil
4、ity 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 e
5、stablished 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
8、phthalate, 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 increa
9、se 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
10、volume 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 b
11、lacks 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 rel
12、ated 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 Balanc
13、e, 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 Dec. 1, 2018. Published January 2019. Originallyapproved in 1976. Last previous
14、 edition approved in 2018 as D3493 18. DOI:10.1520/D3493-18A.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.
15、3Each 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 intern
16、ationally 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 mai
17、ntaining125C 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.) diamete
18、r with 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-te
19、e on 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, ha
20、ving 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
21、the 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 Practice
22、sD1799 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
23、sample 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
24、0.1 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 O
25、pen 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 bla
26、ck 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 clean8
27、50-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
28、 oven 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 near
29、est 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
30、 of 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
31、82, 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 resp
32、onsible 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 informatio
33、n to ASTM International Headquarters.Your comments will receive careful consideration at a meeting of the responsibletechnical committee,1which you may attend.D3493 18a211. Report11.1 Report the following information:11.1.1 Proper identification of the sample,11.1.2 The result obtained from the indi
34、vidual 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 bee
35、n prepared inaccordance with Practice D4483-99. 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
36、testing 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
37、the calculated 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 reje
38、ction testing 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 1.12.4 The results of the precision calculations for this test aregiven in Table 1.
39、The materials are arranged in ascending“mean level” order.12.5 RepeatabilityThe pooled repeatability, r, of this testhas been established as 1.05 105m3/kg (cm3/100 g).Any othervalue in Table 1 may be used as an estimate of repeatability, asappropriate. The difference between two single test results
40、(ordeterminations) 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 appropriat
41、e value fromTable 1 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 s
42、o forth, whichgenerated the two test results.12.6 ReproducibilityThe pooled reproducibility, R,ofthis test method has been established as 3.14 105m3/kg(cm3/100 g). Any other value in Table 1 may be used as anestimate of reproducibility, as appropriate. The differencebetween two single and independen
43、t test results found by twooperators working under the prescribed reproducibility condi-tions in different laboratories on identical test material willexceed the reproducibility on an average of not more than oncein 20 cases in the normal and correct operation of the method.Two single test results p
44、roduced in different laboratories thatdiffer by more than the appropriate value from Table 1 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 tes
45、t value and the reference (true) testproperty value. Reference values do not exist for this testmethod since the value or level of the test property isexclusively defined by the test method. Bias, therefore, cannotbe determined.13. Keywords13.1 carbon black; epoxidized fatty acid ester (EFA) oil;ndi
46、butyl phthalate; oil absorption number of compressedsample; paraffin oilTABLE 1 Precision Parameters for Test Method D3493, Method N/A (Type 1 Precision)AUnits 105m3/kg (cm3/100 g)Material PeriodNumber ofLaboratories(M/H/L)BMeanLevelSr r (r) SR R (R)SRB-9A Mar 2013 70(0/1/0) 67.5 0.35 1.00 1.5 1.10
47、3.12 4.6SRB-9B Mar 2016 75(0/2/0) 90.1 0.45 1.27 1.4 1.24 3.52 3.9SRB-9C Mar/Apr 2014 67(1/1/0) 103.2 0.48 1.36 1.3 1.15 3.24 3.1SRB-9D Mar 2018 67(1/1/0) 34.6 0.21 0.61 1.8 0.84 2.37 6.9SRB-9E Aug 2016 71(0/3/1) 73.2 0.43 1.22 1.7 0.91 2.58 3.5SRB-9F Mar 2015 67(1/1/0) 85.4 0.34 0.97 1.1 1.19 3.37
48、3.9SRB-9G Aug 2017 64(1/2/1) 38.0 0.24 0.67 1.8 1.27 3.59 9.4Average 70.3Pooled Values 0.37 1.05 1.5 1.11 3.14 4.5APreferred precision shown in bold text.BM = number of outliers for Mean; H = number of outliers for High variation; L = number of outliers for Low variation.D3493 18a3ASTM International
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