1、Designation: D5230 091Standard Test Method forCarbon BlackAutomated Individual Pellet Hardness1This standard is issued under the fixed designation D5230; 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 () indicates an editorial change since the last revision or reapproval.1NOTEEditorially corrected Table 1 and Table 2 in June 2010.1. Scope1.1 This test method covers a procedure for measuringindividual pellet hardness
3、 of carbon black by the automatedpellet hardness tester.21.2 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 theresponsi
4、bility 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:3D1511 Test Method for Carbon BlackPellet Size Distri-butionD1799 Practice for Carbon BlackSampl
5、ing PackagedShipmentsD1900 Practice for Carbon BlackSampling Bulk Ship-mentsD4483 Practice for Evaluating Precision for Test MethodStandards in the Rubber and Carbon Black ManufacturingIndustriesE11 Specification for Woven Wire Test Sieve Cloth and TestSieves3. Summary of Test Method3.1 A sample of
6、carbon black is passed through two sievesto isolate a fraction 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 eitherbre
7、ak with a rapid force reduction or the pellet will simplycompress. 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 i
8、s related to several carbonblack characteristics. Among 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.
9、Apparatus5.1 Automated Pellet Hardness Tester,2capable 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 andcons
10、isting of the following major components and character-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 detect
11、the contact shall not exceed 2 cN (2 gf),5.1.2 A means for applying the force at a constant rate,1This test method is under the jurisdiction of ASTM Committee D24 on CarbonBlack and is the direct responsibility of Subcommittee D24.51 on Carbon BlackPellet Properties.Current edition approved Jan. 1,
12、2009. Published February 2009. Originallyapproved in 1992. Last previous edition approved in 2005 as D5230 05. DOI:10.1520/D5230-09E01.2The sole 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,
13、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 aware of alternative suppliers, please provide thisinformation to ASTM International Headquarters. Your comments will receivecareful consideration at a meeting
14、 of the responsible technical committee,1whichyou may attend.3For 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、1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.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 measu
16、red along the axis of the applicationof force.5.1.5 A control device for 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
17、the platen surfaces, and starting the next cycle.5.1.6 An algorithm for determining 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.
18、7 A program for calculating for a specified number ofpellets the data as requested 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 MethodD1511.5.3 Sieves, U.S. Standard No. 12 (1700 m) and No. 14(1
19、400 m) conforming to Specification E11 shall be used totest grades of black that 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 (10
20、00 m) sieves.NOTE 1Pellet size to be tested is 12/14 by program default. Anothersize 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
21、 samples in accordance with Practice D1799 orPractice D1900.7. Calibration7.1 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 poi
22、ntcriteria.7.2.2 Force drop. A decrease of 3 cN (3gf) from themaximum force 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 aredet
23、ermined by agreement between customer and supplier.7.2.5 The following ranges 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
24、.44 mm.8. Procedure8.1 Prepare a sample of carbon black as follows:8.1.1 Stack 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 th
25、e No. 14 sieve, or to testsmaller pellet blacks, stack the No. 16 above the 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 t
26、ransfer the assembly to the mechanical shaker.8.1.5 Allow the sieve assembly to shake for 60 s with thehammer operating.8.2 Remove the assembly from the shaking device. Select asufficiently large sample from the pellets retained on thebottom sieve. The sample size required for testing depends onthe
27、apparatus that is used.8.3 Conduct the test following the instructions in the 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
28、.1.3 Maximum value in centinewtons (gram force)rounded to a whole number9.1.4 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
29、in centinewtons(grams force) rounded to a whole number,9.1.5 Number of pellets 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 D4483. Refer to this practice forterminology and other statist
30、ical details.10.2 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 foracceptance or rejection testing of any gro
31、up 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 1.10.3 A type 1 inter-laboratory precision program was con-ducted as detailed in Table 2. Both repeatability
32、 and reproduc-ibility represent short term (daily) testing conditions. The4The sole source of supply of the special pellet selection 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 infor
33、mation to ASTMInternational Headquarters. Your comments will receive careful consideration at ameeting of the responsible technical committee,1which you may attend.D5230 0912testing was performed using two operators in each laboratoryperforming the test once on each of two days (total of fourtests).
34、 A test result is the average of all the individual pellethardness values obtained in a single determination. Acceptabledifference 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 t
35、his test aregiven in Table 1. The materials are arranged in ascending“mean level” 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
36、single test results (or determina-tions) found on identical test material under 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 mo
37、re than the appropriate value from Table 1 must besuspected of being from different 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 m
38、aterials, samples, etc., which generatedthe two test results.10.6 ReproducibilityThe 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-d
39、ent test results found by two operators working under theprescribed reproducibility 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 resultsp
40、roduced in different laboratories that differ by more than theappropriate value 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 tes
41、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.11. Keywords11.1 carbon black; pellet crush strength; pellet hardnessAST
42、M International takes no position respecting the validity of any patent rights 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 en
43、tirely their own responsibility.This standard is subject to revision at any 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 standardsa
44、nd should be addressed to ASTM International Headquarters. Your comments will 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
45、on Standards, at the address shown below.This standard is copyrighted by ASTM 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
46、at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).TABLE 1 Precision Parameters for D5230 Automated IndividualPellet Hardn
47、ess, (Type 1 Precision)Units cN (gf)WithinLaboratoryBetweenLaboratoryMaterial Mean Level Sr (r) SR (R)N650 23 2 5 4 13SRB D4 (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 D4 (N762) 46September 1997 SRB A5 (N135) 41March 1998 N550 46D5230 0913
