1、Designation: D3493 13Standard 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 and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D1765 Classification System for Carbon Blacks Used inRubber ProductsD1799 Practice for Carbon Black
5、Sampling 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 MethodStandards in the Rubber and Carbo
6、n 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 phthalate, paraffin, or EFA oil is added
7、 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 increase in viscosity. This increased viscosity is
8、transmitted 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 volume of oil per unit mass of carbon blacki
9、s the oil absorption number. Either DBP, paraffin, or EFA oilis acceptable for use with many standard pelleted grades ofN-series carbon blacks found in Classification D1765. COANtesting using paraffin or EFA oil on some specialty blacks andpowder blacks may result in significant differences whencomp
10、ared 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 related tothe processing and vulcanizate properties of
11、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, analytical, 0.01-g sensitivity.1This test method
12、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, 2013. Published August 2013. Originallyapproved in 1976. Last previous edition approved in 2009 as D3493 09. DOI:10.1520/D3
13、493-13.2For 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.3Each apparatus is to be operated and maintained in ac
14、cordance with themanufacturers directions for optimum performance.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States15.2 Oven, gravity-convection type, capable of maintaining125C 6 5C.5.3 Carbon Black Press, capable of compressing a 25-g
15、sample to 165 MPa (24 000 psi).45.4 Absorptometer,5equipped 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 with receiver pan.5.7 Brush, approximately 40 mm (1.5 in.), stiff br
16、istle.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 on Analytical Reagents of the American Chemical Society,where such s
17、pecifications are available.6Other 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, having a density of 1.042 to1.047 mg/m3at 25C and a relative density of
18、1.045 to 1.050at 25C.6.3 Paraffn Oil, having a kinematic viscosity of 10 to34 mm2/s (cSt) at 40C.76.4 Epoxidized Fatty Acid Ester (EFA), meeting the speci-fications listed in Test Method D2414, Table 1. It is recom-mended to store the product at temperatures between 7 and30C. If stored in sealed ori
19、ginal 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.87. Sampling7.1 Samples shall be taken in accordance with PracticesD1799 and D1900.8. Calibration and Standardization8.1 See Test Metho
20、d 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 sample for1hinaspecified oven setat 125C. Cool the sample in a desicc
21、ator 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 g greater than the mass specified insubsection 9.2 of Test Method
22、 D2414.9.3 Compress the sample using either the Chandler or Titanpress.9.4 Chandler Press:9.4.1 Place the bottom seal plate and the compressioncylinder in the hydraulic press. Move the handle of the sealplate to check its position in the support plate. Rotate thecylinder to be certain that it fits o
23、n the seal plate.9.4.2 Place the carbon black sample in the compressioncylinder and insert the piston with the nylon spacer next to thecarbon black. Rotate the piston while pressing it into thecylinder as far as possible by hand.9.4.3 Adjust the alignment of the piston, cylinder, and ramto prevent g
24、alling of the cylinder.9.4.4 Compress the carbon black to approximately 165 MPa(24 000 psi), hold for about 1 s, then release. The exactpressure is determined by measuring the compressed oil. Avalue of the SRB materials and making appropriate adjust-ments. If the values are too high, the pressure is
25、 increased, andif the values are too low, the pressure is lowered.NOTE 2165 MPa (24 000 psi) is equivalent to 131 kN (29 450 lbf) onthe Enerpac gauge GF-20S.9.4.5 Raise the ram to a sufficient height to allow the bottomseal plate to be removed, then lower the ram in order to pressthe piston and samp
26、le through the cylinder and into a sievescreen fitted with a receiver pan.9.4.6 Wipe the piston, cylinder, and seal in order to removecarbon black dust and reassemble the apparatus as described in9.4.1.4The sole source of supply of carbon black presses known to the committee atthis time is Titan Spe
27、cialties, Inc., P.O. Box 2316, Pampa, TX 79066-2316. If youare aware of alternative suppliers, please provide this information to ASTMInternational Headquarters. Your comments will receive careful consideration at ameeting of the responsible technical committee,1which you may attend.5Available from
28、C. W. Brabender Instruments, Inc., 50 E. Wesley St., SouthHackensack, NJ 07606 and from HITEC Luxembourg, 5 Rue de lEglise, L-1458,Luxembourg. The sole source of supply of the apparatus known to the committee atthis time is listed above. If you are aware of alternative suppliers, please provide this
29、information to ASTM International Headquarters. Your comments will receivecareful consideration at a meeting of the responsible technical committee,1whichyou may attend.6Reagent Chemicals, American Chemical Society Specifications , AmericanChemical Society, Washington, DC. For suggestions on the tes
30、ting 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.7The sole source of supply of paraffin oil (Mar
31、col 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
32、responsible technical committee,1whichyou may attend.8The 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 inform
33、ation to ASTM International Headquarters.Your comments will receive careful consideration at a meeting of the responsibletechnical committee,1which you may attend.D3493 1329.4.7 Pass the compressed carbon black through the sievescreen into the receiver.9.4.8 Repeat 9.4.2-9.4.7, compressing the sampl
34、e a total offour times. Retain the sample from 9.4.7 after the fourthcompression. Proceed to 9.6.9.5 Titan Press :9.5.1 Lower the cylinder piston by pressing the left handlever downward, then pour the carbon black sample into thecylinder.9.5.2 Close and latch the door of the press. Compress thesampl
35、e by operating the ram using a downward movement ofthe right hand lever, until the preset gauge pressure reachesapproximately 11 MPa (1550 psi). Release immediately. Theexact pressure is determined by measuring the oil absorption ofthe compressed SRB materials and making appropriate adjust-ments. If
36、 the values are too high, the pressure is increased, andif the values are too low, the pressure is lowered.9.5.3 Raise the ram until it is level with the top of theconical collar placed on top of the cylinder.9.5.4 Raise the cylinder piston until the compressed sampleis broken by contact with the ra
37、ised ram.The conical collar willretain the sample.9.5.5 Break up the sample with a spatula, lower the cylinderpiston, and allow the sample to fall back into cylinder. Ifnecessary, brush the inside of the collar to return all of thecarbon black to the cylinder.9.5.6 Repeat 9.5.2-9.5.5 an additional t
38、hree times, for a totalof four compression cycles.9.5.7 Remove the sample and pass it through a 850-msieve (sieve #20).9.6 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.NO
39、TE 3If the compressed sample is not to be tested within 15 minafter compression, it should be stored in a desiccator or dried for1hinthespecified oven set at 125C prior to testing.10. Calculation10.1 Calculate the oil absorption number, compressedsample, to the nearest 0.1 105m3/kg (cm3/100 g) as fo
40、llows:Oil absorption number, compressed sample, 1025m3/kg5AB3100where:A = volume of oil used, cm3, andB = mass of tested sample, g.11. Report11.1 Report the following information:11.1.1 Proper identification of the sample,11.1.2 The result obtained from the individual determina-tion is reported to t
41、he nearest 0.1 105m3/kg (cm3/100 g),11.1.3 Oil (DBP or paraffin), 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 prepared inaccordance with Practice D4483. Refer to this practic
42、e forterminology and other statistical details.12.2 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 program de-scribed below. The precision parameters should not be used foracceptan
43、ce or rejection 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 1.12.3 A type 1 inter-laboratory precision program was con-ducted as detai
44、led in Table 1. Both repeatability and reproduc-ibility represent short-term (daily) testing conditions. Thetesting was performed using two operators in each laboratoryperforming the test once on each material on each of two days(total of four tests). A test result is the value obtained from asingle
45、 determination. Acceptable difference values were notmeasured. The between operator component of variation isincluded in the calculated values for r and R.12.4 The results of the precision calculations for this test aregiven in Table 1. The materials are arranged in ascending“mean level” order.12.5
46、RepeatabilityThe pooled absolute repeatability, r,ofthis test has been established as 2.01 105m3/kg (cm3/100 g).Any other value in Table 1 may be used as an estimate ofrepeatability, as appropriate. The difference between two singletest results (or determinations) found on identical test materialund
47、er the repeatability conditions prescribed for this test willexceed the repeatability on an average of not more than once in20 cases in the normal and correct operation of the method.Two single test results that differ by more than the appropriatevalue from Table 1 must be suspected of being from di
48、fferentpopulations and some appropriate action taken.NOTE 4Appropriate 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, whichgenerated the two test results.12.6 Repr
49、oducibilityThe pooled absolute reproducibility,R, of this test has been established as 4.03 105m3/kg (cm3/TABLE 1 Precision Parameters for D3493 Oil Absorption Numberof Compressed Sample, (Type 1 Precision)AUnitsNumberofLaboratories105m3/kg (cm3/100 g)Material Mean Level Sr r SR RSRB D6 (N762) 13 60.2 0.53 1.51 1.23 3.48SRB C6 (N326) 13 68.1 0.53 1.51 1.04 2.96SRB E6 (N660) 13 76.0 0.83 2.34 1.95 5.51SRB F6 (N683) 13 88.6 0.86 2.42 1.53 4.34SRB B6 (N220) 15 98.5 0.60 1.71 1.36 3.86SRB A6 (N134) 15 101.0 0.82 2.33 1.24 3.50Averag
