1、Designation: D5230 12 D5230 12aStandard 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 rev
2、ision. 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 t
3、ester.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 Blac
5、kSampling 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 isol
6、ate a fraction of uniform size. The most spherical pellets fromthis portion are selected and placed into the tester. The individual pellets are pressed against a platen with a load cell for measuringforce. As pressure is applied the pellet will either break with a rapid force reduction or the pellet
7、 will simply compress. Theindividual pellet hardness is the maximum force prior to a force reduction of at least 3 cN or the maximum force required tocompress the pellet to 90 %, whichever comes first.4. Significance and Use4.1 Individual pellet hardness is related to several carbon black characteri
8、stics. 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 Automated Pellet Hardness Te
9、ster, 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 following major components
10、 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 July 1, 2012Aug. 15, 2012. Published October 2012. Originally approved in 1992. La
11、st previous edition approved in 20102012 asD5230 10.D5230 12. DOI: 10.1520/D5230-12.10.1520/D5230-12A.2 The sole source of supply of the Concarb Titan Automated Pellet Hardness Tester known to the committee at this time is Jaron Technologies LLC, 2338 Duncan, Pampa,TX 79065, E-mail: http:/. The HITE
12、C 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 carefulconsideration at a meeting of t
13、he responsible technical committee,1 which you may attend.3 For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.
14、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 recommends that users consult prior edi
15、tions 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 automatic loading of a pellet
16、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 at a constant rate,5.1.3 A mea
17、ns 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 instrument through the test cycle tha
18、t 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 individual test end point (determina
19、tion) 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 Section 9, and5.1.8 A means for id
20、entifying, 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 be segregated in a 12/+14 fract
21、ion. 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.5.5 Special Pellet Selection Tray, 4 (shallow container)
22、, flat and approximately 300 mm (12 in.) long.6. Sampling6.1 Take samples 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 p
23、ellet diameter to 90 % of the original value is one of two end point criteria.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 pel
24、lets, critical applications, 50 pellets. Critical applications aredetermined 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 F
25、or 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 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
26、to screen several samples simultaneously.8.1.2 Stack the No. 12 above the 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 mech
27、anical shaker.8.1.4 Allow the sieve assembly to shake for 60 s with the 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 Co
28、nduct the test following the instructions in the equipment 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) rounded to the nearest millinewton (nearest 0.1 g force),9.1.3 Maximum value in centine
29、wtons (gram force) rounded to a whole number9.1.4 Number of pellets tested, andD5230 12a29.1.5 Size of sieves used to prepare the sample.10. Precision and Bias10.1 These precision statements have been prepared in accordance with Practice D4483. Refer to this practice for terminologyand other statist
30、ical details.10.2 The precision results in this precision and bias section 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 gro
31、up of materials without documentation that they are applicable to those 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
32、and reproducibilityrepresent short term (daily) testing conditions. The 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 determ
33、ination. Acceptable difference values were not measured. The between operator 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 Repea
34、tabilityThe pooled relative repeatability, (r), of this test has been established 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
35、conditions prescribed for this test will exceed the repeatability on an 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
36、 and some appropriate action taken.NOTE 2Appropriate action may be an investigation 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 re
37、lative reproducibility, (R), of this test has been established as 14 %. 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 condition
38、s in different laboratories on identical testmaterial will exceed the reproducibility 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
39、 1must be suspected of being from different populations and some appropriate 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 thi
40、s test method since the value or level of the test property is exclusively 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 Precisi
41、on)Units cN (gf) WithinLaboratory BetweenLaboratoryMaterial 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 14D5230 12a3ASTM International takes no position respecting the validity of any
42、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 entirely their own responsibility.This standard is subject to revis
43、ion 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 standardsand should be addressed to ASTM International Headquarters. Your c
44、omments 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 on Standards, at the address shown below.This standard is copyrig
45、hted 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 at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (
46、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/).4 The sole source of supply of the special pellet selection tray known to the committee at this time is Titan Specialties, Inc., P.O. Bo
47、x 2316, Pampa, TX 79065. If youare aware of alternative suppliers, please provide this information to ASTM International Headquarters. Your comments will receive careful consideration at a meeting ofthe responsible technical committee,1 which you may attend.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 12a4
