1、Designation: D5230 12aD5230 13Standard 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 revi
2、sion. 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 a procedure for measuring individual pellet hardness of carbon black by the automated pellethardness te
3、ster.21.2 The values stated in SI units are to be regarded as the standard. The values in parentheses are for information only.1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish
4、appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:3D1511 Test Method for Carbon BlackPellet Size DistributionD1799 Practice for Carbon BlackSampling Packaged ShipmentsD1900 Practice for Carbon Black
5、Sampling Bulk ShipmentsD4483 Practice for Evaluating Precision for Test Method Standards in the Rubber and Carbon Black Manufacturing IndustriesE11 Specification for Woven Wire Test Sieve Cloth and Test Sieves3. Summary of Test Method3.1 A sample of carbon black is passed through two sieves to isola
6、te a fraction of uniform size. The most spherical Anappropriate amount of pellets from this portion areis selected and placed into the tester. The individual pellets are pressed againsta platen with a load cell for measuring force. As pressure is applied the pellet will either break with a rapid for
7、ce reduction or thepellet will simply compress. The individual pellet hardness is the maximum force prior to a force reduction of at least 3 cN or themaximum force required to compress the pellet to 90 %, whichever comes first.4. Significance and Use4.1 Individual pellet hardness is related to sever
8、al carbon black characteristics.Among these are mass strength and attrition. Thesubsequent level of dispersion obtained in some mixed compounds containing the carbon black may be affected by pellet hardness.Acceptable pellet hardness must be agreed to by the user and the producer.5. Apparatus5.1 Aut
9、omated Pellet Hardness Tester, 2 capable of achieving an absolute measuring accuracy of 62 cN (2 gf) for the forcemeasurement and 60.1 mm for the diameter measurement and a relative accuracy of 60.5 cN (0.5 gf) for the force measurementand 0.02 mm for the diameter measurement and consisting of the f
10、ollowing major components and characteristics.1 This test method is under the jurisdiction of ASTM Committee D24 on Carbon Black and is the direct responsibility of Subcommittee D24.51 on Carbon Black PelletProperties.Current edition approved Aug. 15, 2012Jan. 1, 2013. Published October 2012February
11、 2013. Originally approved in 1992. Last previous edition approved in 2012 asD5230 12.D5230 12a. DOI: 10.1520/D5230-12A.10.1520/D5230-13.2 The sole source of supply of the Concarb TitanAutomated Pellet Hardness Tester known to the committee at this time is Jaron Technologies LLC, 2338 Duncan, Pampa,
12、TX 79065, E-mail: http:/. The HITEC IPHT is available from HITEC Luxembourg, 5 rue de L Eglise, L-1458, Luxembourg, E-mail: infohitec.lu,http:/www.hitec.lu/. If you are aware of alternative suppliers, please provide this information to ASTM International Headquarters. Your comments will receive care
13、fulconsideration at a meeting of the responsible technical committee,1 which you may attend.3 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Su
14、mmary page on the ASTM website.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommen
15、ds that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States15.1.1 A means for
16、 automatic loading of a pellet on the transport platen for transporting the pellet so as to contact the secondplaten with a minimum force. Typically one platen contains a force measuring device. The required force to detect the contact shallnot exceed 2 cN (2 gf),5.1.2 A means for applying the force
17、 at a constant rate,5.1.3 A means for transporting the pellet so to minimize its movement during the application of force.5.1.4 A means for measuring the diameter of the individual pellet under test as measured along the axis of the application offorce.5.1.5 A control device for directing the instru
18、ment through the test cycle that includes crushing the pellet under controlledconditions, measuring and storing the results of the initial diameter and crush force determinations, cleaning the fragments fromthe platen surfaces, and starting the next cycle.5.1.6 An algorithm for determining the indiv
19、idual test end point (determination) as the maximum observed force prior to thefirst occurrence of either a specified reduction in diameter or a specified reduction in force from the maximum force observed,5.1.7 A program for calculating for a specified number of pellets the data as requested in Sec
20、tion 9, and5.1.8 A means for identifying, viewing, printing, and storing the data in an ASCII file.5.2 Mechanical Sieve Shaker, conforming to Test Method D1511.5.3 Sieves, U.S. Standard No. 12 (1700 m) and No. 14 (1400 m) conforming to Specification E11 shall be used to test gradesof black that can
21、be segregated in a 12/+14 fraction. For grades of black that are too small to be retained on a No. 14 sieve, i.e.,acetylene and thermal blacks, it is acceptable to test with U.S. Standard No. 16 (1180 m) and No. 18 (1000 m) sieves.5.4 Bottom-Receiver Pan and Top-Sieve Cover.6. Sampling6.1 Take sampl
22、es in accordance with Practice D1799 or Practice D1900.7. Calibration7.1 Calibrate force and diameter measurement following the manufacturers instructions.7.2 Instrument Parameters:7.2.1 Crush diameter, 0.90. A reduction of the pellet diameter to 90 % of the original value is one of two end point cr
23、iteria.7.2.2 Force drop. A decrease of 3 cN (3gf) from the maximum 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, 20 pellets, critical applications, 50 pellets. Critical applications aredeter
24、mined by agreement between customer and supplier.7.2.5 The following ranges of acceptable pellet diameters were established to minimize the number of pellets rejected due toinstrument 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.
25、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 to top: bottom receiver pan, No. 14, and No. 12.NOTE 1It is permissible to use multiples of sieve stacks to screen several samples simultaneously.8.1.2 Stack the No. 12 above t
26、he No. 14 sieve, or to test smaller pellet blacks, stack the No. 16 above the No. 18 sieve withthe reciever pan on the bottom.8.1.3 Transfer the sample to the No. 12 screen, install the cover and transfer the assembly to the mechanical shaker.8.1.4 Allow the sieve assembly to shake for 60 s with the
27、 hammer operating.8.2 Remove the assembly from the shaking device. Select a sufficiently large sample from the pellets retained on the bottomsieve. The sample size required for testing depends on the apparatus that is used.8.3 Conduct the test following the instructions in the equipment operation ma
28、nual.9. Report9.1 Report the following information:9.1.1 Proper identification of the sample,9.1.2 Average value in centinewtons (gram force) rounded to the nearest millinewton (nearest 0.1 g force),9.1.3 Maximum value in centinewtons (gram force) rounded to a whole number9.1.4 Number of pellets tes
29、ted, and9.1.5 Size of sieves used to prepare the sample.D5230 13210. Precision and Bias10.1 These precision statements have been prepared in accordance with Practice D4483. Refer to this practice for terminologyand other statistical details.10.2 The precision results in this precision and bias secti
30、on give an estimate of the precision of this test method with thematerials used in the particular interlaboratory program described below. The precision parameters should not be used foracceptance or rejection testing of any group of materials without documentation that they are applicable to those
31、particularmaterials and the specific testing protocols of the test method. Any appropriate value may be used from Table 1.10.3 A type 1 inter-laboratory precision program was conducted as detailed in Table 2. Both repeatability and reproducibilityrepresent short term (daily) testing conditions. The
32、testing was performed using two operators in each laboratory performing thetest once on each of two days (total of four tests). A test result is the average of all the individual pellet hardness values obtainedin a single determination. Acceptable difference values were not measured. The between ope
33、rator component of variation isincluded in the calculated values for r and R.10.4 The results of the precision calculations for this test are given in Table 1. The materials are arranged in ascending “meanlevel” order.10.5 RepeatabilityThe pooled relative repeatability, (r), of this test has been es
34、tablished as 5 %. Any other value in Table 1may be used as an estimate of repeatability, as appropriate. The difference between two single test results (or determinations) foundon identical test material under the repeatability conditions prescribed for this test will exceed the repeatability on an
35、average ofnot more than once in 20 cases in the normal and correct operation of the method. Two single test results that differ by more thanthe appropriate value from Table 1 must be suspected of being from different populations and some appropriate action taken.NOTE 2Appropriate action may be an in
36、vestigation of the test method procedure or apparatus for faulty operation or the declaration of a significantdifference in the two materials, samples, etc., which generated the two test results.10.6 ReproducibilityThe pooled relative reproducibility, (R), of this test has been established as 14 %.
37、Any other value inTable 1 may be used as an estimate of reproducibility, as appropriate. The difference between two single and independent testresults found by two operators working under the prescribed reproducibility conditions in different laboratories on identical testmaterial will exceed the re
38、producibility on an average of not more than once in 20 cases in the normal and correct operation ofthe method. Two single test results produced in different laboratories that differ by more than the appropriate value from Table 1must be suspected of being from different populations and some appropr
39、iate investigative or technical/commercial action taken.10.7 BiasIn test method terminology, bias is the difference between an average test value and the reference (true) test propertyvalue. Reference values do not exist for this test method since the value or level of the test property is exclusive
40、ly defined by thetest method. Bias, therefore, cannot be determined.11. Keywords11.1 carbon black; pellet crush strength; pellet hardnessTABLE 1 Precision Parameters for D5230 Automated IndividualPellet Hardness, (Type 1 Precision)Units cN (gf) WithinLaboratory BetweenLaboratoryMaterial Mean Level S
41、r (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 14D5230 133ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this stand
42、ard. 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 time by the responsible technical committee and must be review
43、ed 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 will receive careful consideration at a meeting of theresponsible
44、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 ASTM International, 100 Barr Harbor Drive, PO Box C700, West Consh
45、ohocken, 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 through the ASTM website(www.astm.org). Permission rights to p
46、hotocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).TABLE 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 134
