1、Designation: D 5230 05Standard Test Method forCarbon BlackAutomated Individual Pellet Hardness1This standard is issued under the fixed designation D 5230; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A
2、 number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers a procedure for measuringindividual pellet hardness of carbon black by the automatedpellet hardness tester.21
3、.2 The values stated in SI units are to be regarded as thestandard. The values in parentheses are for information only.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 standard to establish appro-pri
4、ate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:3D 1511 Test Method for Carbon BlackPellet Size Distri-butionD 1799 Practice for Carbon BlackSampling PackagedShipmentsD 1900 Practice for Carbon BlackSam
5、pling Bulk Ship-mentsD 4483 Practice for Evaluating Precision for Test MethodStandards in the Rubber and Carbon Black ManufacturingIndustriesE11 Specification for Wire Cloth and Sieves for TestingPurposes3. Summary of Test Method3.1 A sample of carbon black is passed through two sievesto isolate a f
6、raction of uniform size. The most spherical pelletsfrom this portion are selected and placed into the tester. Theindividual pellets are pressed against a platen with a load cellfor measuring force.As pressure is applied the pellet will eitherbreak with a rapid force reduction or the pellet will simp
7、lycompress. The individual pellet hardness is the maximum forceprior to a force reduction of at least 3 cN or the maximum forcerequired to compress the pellet to 90 %, whichever comes first.4. Significance and Use4.1 Individual pellet hardness is related to several carbonblack characteristics. Among
8、 these are mass strength andattrition. The subsequent level of dispersion obtained in somemixed compounds containing the carbon black may be affectedby pellet hardness. Acceptable pellet hardness must be agreedto by the user and the producer.5. Apparatus5.1 Automated Pellet Hardness Tester,2capable
9、of achiev-ing an absolute measuring accuracy of 62 cN (2 gf) for theforce measurement and 60.1 mm for the diameter measure-ment and a relative accuracy of 60.5 cN (0.5 gf) for the forcemeasurement and 0.02 mm for the diameter measurement andconsisting of the following major components and character-
10、istics.5.1.1 A means for automatic loading of a pellet on thetransport platen for transporting the pellet so as to contact thesecond platen with a minimum force. Typically one platencontains a force measuring device. The required force to detectthe contact shall not exceed 2 cN (2 gf),5.1.2 A means
11、for applying the force at a constant rate,5.1.3 A means for transporting the pellet so to minimize itsmovement during the application of force.5.1.4 A means for measuring the diameter of the individualpellet under test as measured along the axis of the applicationof force.5.1.5 A control device for
12、directing the instrument throughthe test cycle that includes crushing the pellet under controlledconditions, measuring and storing the results of the initialdiameter and crush force determinations, cleaning the frag-ments from the platen surfaces, and starting the next cycle.1This test method is und
13、er the jurisdiction of ASTM Committee D24 on CarbonBlack and is the direct responsibility of Subcommittee D24.51 on Carbon BlackPellet Properties.Current edition approved Dec. 1, 2005. Published January 2006. Originallyapproved in 1992. Last previous edition approved in 2004 as D 5230 04e1.2The sole
14、 source of supply of the Concarb Titan Automated Pellet HardnessTester known to the committee at this time is Titan Specialties, Inc., P.O. Box 2316,Pampa, TX 79065, E-mail: . The HITEC IPHT isavailable from HITEC Luxembourg, 5 rue de L Eglise, L-1458, Luxembourg,E-mail: infohitec.lu. If you are awa
15、re 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.3For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact AST
16、M Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5.1.6 An algorithm for determ
17、ining the individual test endpoint (determination) as the maximum observed force prior tothe first occurrence of either a specified reduction in diameteror a specified reduction in force from the maximum forceobserved,5.1.7 A program for calculating for a specified number ofpellets the data as reque
18、sted in Section 9, and5.1.8 Ameans for identifying, viewing, printing, and storingthe data in an ASCII file.5.2 Mechanical Sieve Shaker, conforming to Test MethodD 1511.5.3 Sieves, U.S. Standard No. 12 (1700 m) and No. 14(1400 m) conforming to Specification E11shall be used totest grades of black th
19、at can be segregated in a 12/+14fraction. For grades of black that are too small to be retained ona No. 14 sieve, i.e., acetylene and thermal blacks, it isacceptable to test with U.S. Standard No. 16 (1180 m) andNo. 18 (1000 m) sieves.NOTE 1Pellet size to be tested is 12/14 by program default. Anoth
20、ersize may be selected if desired by pressing menu item “6.”5.4 Bottom-Receiver Pan and Top-Sieve Cover.5.5 Special Pellet Selection Tray,4(shallow container), flatand approximately 300 mm (12 in.) long.6. Sampling6.1 Take samples in accordance with Practice D 1799 orPractice D 1900.7. Calibration7.
21、1 Calibrate force and diameter measurement following themanufacturers instructions.7.2 Instrument Parameters:7.2.1 Crush diameter, 0.90. A reduction of the pellet diam-eter to 90 % of the original value is one of two end pointcriteria.7.2.2 Force drop. A decrease of 3 cN (3gf) from themaximum force
22、observed is one of two end point criteria.7.2.3 Rate of piston movement during crush, 0.125 mm/s.7.2.4 Number of pellets tested; normal applications, 20pellets, critical applications, 50 pellets. Critical applications aredetermined by agreement between customer and supplier.7.2.5 The following range
23、s of acceptable pellet diameterswere established to minimize the number of pellets rejecteddue to instrument variation and non-spherical pellets.7.2.5.1 For a 12/+14 fraction, 1.311.93 mm.7.2.5.2 For a 16/+18 fraction, 0.801.44 mm.8. Procedure8.1 Prepare a sample of carbon black as follows:8.1.1 Sta
24、ck the sieves in the following order from bottom totop: bottom receiver pan, No. 14, and No. 12.NOTE 2It is permissible to use multiples of sieve stacks to screenseveral samples simultaneously.8.1.2 Stack the No. 12 above the No. 14 sieve, or to testsmaller pellet blacks, stack the No. 16 above the
25、No. 18 sievewith the reciever pan on the bottom.8.1.3 Place the sample in the top sieve and install the cover.Transfer the assembly to the shaking device.8.1.4 Transfer the sample to the No. 12 screen, install thecover and transfer the assembly to the mechanical shaker.8.1.5 Allow the sieve assembly
26、 to shake for 60 s with thehammer operating.8.2 Remove the assembly from the shaking device. Selectthe more spherical pellets retained on the bottom sieve.8.3 Remove the assembly from the shaking device. Selectthe more spherical pellets retained on the No. 14 sieve.8.3.1 The more spherical pellets m
27、ay be selected by use ofa special pellet selection tray. Pour approximately2gofpelletsinto the wide end of the tray, tilt the tray slightly to cause themore spherical pellets to roll to the narrow end. Collect themore spherical pellets for testing.8.4 Conduct the test following the instructions in t
28、he equip-ment operation manual.9. Report9.1 Report the following information:9.1.1 Proper identification of the sample,9.1.2 Average value in centinewtons (gram force) roundedto the nearest millinewton (nearest 0.1 g force),9.1.3 Maximum value in centinewtons (gram force)rounded to a whole number9.1
29、.4 In critical applications (testing 50 or more pellets) andby agreement between customer and supplier, the average ofthe highest 5 pellets, or the average ofx%oftheindividual testvalues (10 % being typical), can be reported in centinewtons(grams force) rounded to a whole number,9.1.5 Number of pell
30、ets tested, and9.1.6 Size of sieves used to prepare the sample.10. Precision and Bias10.1 These precision statements have been prepared inaccordance with Practice D 4483. Refer to this practice forterminology and other statistical details.10.2 The precision results in this precision and bias section
31、give 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 documentation that they are applicable to those par
32、-ticular materials and the specific testing protocols of the testmethod. Any appropriate value may be used from Table 1.10.3 A type 1 inter-laboratory precision program was con-ducted as detailed in Table 2. Both repeatability and reproduc-ibility represent short term (daily) testing conditions. The
33、testing was performed using two operators in each laboratoryperforming the test once on each of two days (total of fourtests). A test result is the average of all the individual pellethardness values obtained in a single determination. Acceptable4The sole source of supply of the special pellet selec
34、tion tray known to thecommittee at this time is Titan Specialties, Inc., P.O. Box 2316, Pampa, TX 79065.If you are aware of alternative suppliers, please provide this information to ASTMInternational Headquarters. Your comments will receive careful consideration at ameeting of the responsible techni
35、cal committee,1which you may attend.D5230052difference values were not measured. The between operatorcomponent of variation is included in the calculated values forr and R.10.4 The results of the precision calculations for this test aregiven in Table 1. The materials are arranged in ascending“mean l
36、evel” order.10.5 RepeatabilityThe pooled relative repeatability, (r), ofthis test has been established as 5 %. Any other value in Table1 may be used as an estimate of repeatability, as appropriate.The difference between two single test results (or determina-tions) found on identical test material un
37、der the repeatabilityconditions prescribed for this test will exceed the repeatabilityon an average of not more than once in 20 cases in the normaland correct operation of the method. Two single test results thatdiffer by more than the appropriate value from Table 1 must besuspected of being from di
38、fferent populations and some appro-priate 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, etc., which generatedthe two test results.10.6 Reproducib
39、ilityThe pooled relative reproducibility,(R), of this test has been established as 14 %. Any other valuein Table 1 may be used as an estimate of reproducibility, asappropriate. The difference between two single and indepen-dent test results found by two operators working under theprescribed reproduc
40、ibility conditions in different laboratorieson identical test material will exceed the reproducibility on anaverage of not more than once in 20 cases in the normal andcorrect operation of the method. Two single test resultsproduced in different laboratories that differ by more than theappropriate va
41、lue from Table 1 must be suspected of beingfrom different populations and some appropriate investigativeor technical/commercial action taken.10.7 BiasIn test method terminology, bias is the differ-ence between an average test value and the reference (true) testproperty value. Reference values do not
42、 exist for this testmethod since the value or level of the test property isexclusively defined by the test method. Bias, therefore, cannotbe determined.11. Keywords11.1 carbon black; pellet crush strength; pellet hardnessASTM International takes no position respecting the validity of any patent righ
43、ts asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any
44、time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments wil
45、l receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by AST
46、M International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or
47、 through the ASTM website(www.astm.org).TABLE 1 Precision Parameters for D 5230 Automated IndividualPellet Hardness, (Type 1 Precision)Units cN (gf)Material Mean Level Sr (r) SR (R)N650 23 2 5 4 13SRB N762 24 2 5 6 16IRB#6 (N330) 30 2 6 4 13SRB A5 (N135) 31 2 5 5 13N550 32 2 6 5 15Average 28Pooled Values 2 5 5 14TABLE 2 Interlaboratory Precision ProgramNominal Test Period Material Number of LaboratoriesMarch 1996 N650 50October 1996 IRB#6 (N330) 39March 1997 SRB N762 46September 1997 SRB A5 (N135) 41March 1998 N550 46D5230053
