1、Designation: D 3493 09Standard Test Method forCarbon BlackOil Absorption Number of CompressedSample (COAN)1This standard is issued under the fixed designation D 3493; 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 t
3、he 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 theresponsibi
4、lity 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:2D 1765 Classification System for Carbon Blacks Used inRubber ProductsD 1799 Practice for Carbon B
5、lackSampling PackagedShipmentsD 1900 Practice for Carbon BlackSampling Bulk Ship-mentsD 2414 Test Method for Carbon BlackOil AbsorptionNumber (OAN)D 4821 Guide for Carbon BlackValidation of TestMethod Precision and BiasD 4483 Practice for Evaluating Precision for Test MethodStandards in the Rubber a
6、nd 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 phthalate or paraffin oil is add
7、ed by means ofa constant-rate buret to the compressed sample of carbon blackin the mixer chamber of an absorptometer. As the sampleabsorbs the oil, the mixture changes from a free-flowing stateto one of a semiplastic agglomeration, with an accompanyingincrease in viscosity. This increased viscosity
8、is transmitted tothe torque-sensing system of the absorptometer. When theviscosity of the mixture reaches a predetermined torque level,the absorptometer and buret will simultaneously shut off. Thevolume of oil added is read from the direct reading buret. Thevolume of oil per unit mass of carbon blac
9、k is the oilabsorption number. Either DBP or paraffin oil is acceptable foruse with many standard pelleted grades of N-series carbonblacks found in Classification D 1765. COAN testing usingparaffin oil on some specialty blacks and powder blacks mayresult in significant differences when compared to C
10、OANtesting using DBP oil. Referee testing between suppliers andusers should use DBP oil until such time that precision data isavailable for paraffin oil.4. Significance and Use4.1 The oil absorption number of a carbon black is related tothe processing and vulcanizate properties of rubber compoundsco
11、ntaining 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.5.2 Oven, gravity-convection type, c
12、apable of maintaining125C 6 5C.5.3 Carbon Black Press, capable of compressing a 25-gsample to 165 MPa (24 000 psi).41This 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 approve
13、d May 1, 2009. Published May 2009. Originallyapproved in 1976. Last previous edition approved in 2007 as D 3493 07.2For 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 t
14、he standards Document Summary page onthe ASTM website.3Each apparatus is to be operated and maintained in accordance with themanufacturers directions for optimum performance.4The sole source of supply of carbon black presses known to the committee atthis time is Titan Specialties, Inc., P.O. Box 231
15、6, 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.1Copyright ASTM International, 100 Barr Harb
16、or Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5.4 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,
17、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 on Analytical Reagents of the
18、 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 permit its use without lessening theaccuracy of the determination.6.2 n-Dibutyl Phthalate, having a density of 1.042 to1.047
19、 mg/m3at 25C and a relative density of 1.045 to 1.050at 25C.6.3 Paraffin oil, having a kinematic viscosity of 10 to34 mm2/s (cSt) at 40C.76.4 ASTM D24 Standard Reference Blacks, SRB.87. Sampling7.1 Samples shall be taken in accordance with PracticesD 1799 and D 1900.8. Calibration and Standardizatio
20、n8.1 See Test Method D 2414.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 D 4821.9. Procedure9.1 Dry an adequate sample for1hinaspecified oven setat 125C. Cool t
21、he 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 D 2414. The desired sample mass to be compressedwill weigh 5 6 0.1 g greater than the mass specified insubsect
22、ion 9.2 of Test Method D 2414.9.3 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
23、 certain that it fits on 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, cylind
24、er, and ramto prevent galling 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 to
25、o high, the pressure is 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 p
26、ressthe piston and sample 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 in9.4.1.9.4.7 Pass the compressed carbon black through the sievescreen into the rec
27、eiver.9.4.8 Repeat 9.4.2-9.4.7, compressing the sample 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 Clos
28、e and latch the door of the press. Compress thesample 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 S
29、RB materials and making appropriate adjust-ments. If 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 t
30、he compressed sampleis broken by contact with the raised 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. If5Available from C. W. Brabender Instruments, Inc., 50 E. Wesley St., SouthHacke
31、nsack, 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 thisinformation to ASTM International Headquarters. Your comments w
32、ill 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 testing of reagents notlisted by the American Chemical Society, se
33、e 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 (Marcol 82, which has beendemonstrated to provide comparable result
34、s 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 responsible technical committee,1whichyou may attend.8The sole
35、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 to ASTM International Headquarters.Your comments will rec
36、eive careful consideration at a meeting of the responsibletechnical committee,1which you may attend.D3493092necessary, 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 three times, for a totalof four compression cycles.9.5.7 Remov
37、e 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 D 2414. Use the samesample masses as recommended in subsection 9.2 of TestMethod D 2414.NOTE 3If the compressed sample is not to be tested within 15
38、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 follows:Oil absorption number, compressed sample, 1025m3/kg5A
39、B3 100where: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 the nearest 0.1 105m3/kg (cm3/100 g),11.1.3 Oil (DBP or par
40、affin), and11.1.4 Method for end-point determination (ProcedureA, B,or C on Standardization in Test Method D 2414).12. Precision and Bias12.1 These precision statements have been prepared inaccordance with Practice D 4483. Refer to this practice forterminology and other statistical details.12.2 The
41、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 foracceptance or rejection testing of any group of materialswithout
42、 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 detailed in Table 1. Both repeatability and reproduc-ibility
43、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 determination. Acceptable difference values were notmea
44、sured. 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 RepeatabilityThe pooled absolute repeatability, r,ofthis
45、 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 materialunder the repeatability conditions prescribed for this test
46、 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 differentpopulations and some appropriate action taken.NOT
47、E 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 ReproducibilityThe pooled absolute reproducibility,R, of thi
48、s test has been established as 4.03 105m3/kg (cm3/100 g). Any other value in Table 1 may be used as an estimateof reproducibility, as appropriate. The difference between twosingle and independent test results found by two operatorsworking under the prescribed reproducibility conditions indifferent l
49、aboratories 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 laboratories that differ bymore 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 differ-ence between an average test value and the reference (true) testproper
