1、Designation: D5230 141Standard 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.1NOTECorrected 1.1 and 5.1 editorially in October 2016.1. Scope1.1 This test method covers a procedure for measuringindividual pellet hardness of c
3、arbon black by the automatedpellet hardness tester.1.2 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
4、 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:2D1511 Test Method for Carbon BlackPellet Size Distri-butionD1799 Practice for Carbon BlackSampling Pa
5、ckagedShipmentsD1900 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 carbon
6、 black is passed through two sievesto isolate a fraction of uniform size. An appropriate amount ofpellets from this portion is selected and placed into the tester.The individual pellets are pressed against a platen with a loadcell for measuring force. As pressure is applied the pellet willeither bre
7、ak with a rapid force reduction or the pellet willsimply compress. The individual pellet hardness is the maxi-mum 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
8、is 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, capable of achievingan absolute measuring accuracy of 62 cN (2 gf) for the forcemeasurement and 60.1 mm for the diameter measurement anda relative accuracy of 60.5 cN (0.5 gf) for the force measure-ment and 0.02 mm for the diameter measurement and cons
10、ist-ing of the following major components and characteristics.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,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
12、 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 the platen surface
13、s, 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,1This test method is u
14、nder the jurisdiction of ASTM Committee D24 on CarbonBlack and is the direct responsibility of Subcommittee D24.51 on Carbon BlackPellet Properties.Current edition approved Sept. 1, 2014. Published October 2014. Originallyapproved in 1992. Last previous edition approved in 2013 as D5230 13. DOI:10.1
15、520/D5230-14E01.2For 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 the standards Document Summary page onthe ASTM website.Copyright ASTM International, 100 Barr Harbor
16、 Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States15.1.7 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 t
17、o Test MethodD1511.5.3 Sieves, U.S. Standard No. 12 (1700 m) and No. 14(1400 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,
18、 it isacceptable to test with U.S. Standard No. 16 (1180 m) andNo. 18 (1000 m) sieves.5.4 Bottom-Receiver Pan and Top-Sieve Cover.6. Sampling6.1 Take samples in accordance with Practice D1799 orPractice D1900.7. Calibration7.1 Calibrate force and diameter measurement following themanufacturers instr
19、uctions.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 observed is one of two end point criteria.7.2.3 Rate of piston movement dur
20、ing 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 ranges of acceptable pellet diameterswere established to minimize the number of
21、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 Stack the sieves in the following order from bottom totop: bottom receiver pan
22、, No. 14, and No. 12.NOTE 1It 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 No. 18 sievewith the reciever pan on the bottom.8.1.3 Transfer the sample t
23、o the No. 12 screen, install thecover and transfer the assembly to the mechanical shaker.8.1.4 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 samp
24、le size required for testing depends onthe 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
25、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 tested, and9.1.5 Size of sieves used to prepare the sample.10. Precision and Bias10.1 These precision statements have been prepared inaccordance with Practice D4
26、483. Refer to this practice forterminology and other statistical 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 shou
27、ld not be used foracceptance or rejection testing of any group of materialswithout documentation that they are applicable to those par-ticular materials and the specific testing protocols of the testmethod.10.3 A type 1 inter-laboratory precision program was con-ducted as detailed in Tables 1-4. Bot
28、h repeatability andreproducibility represent short term (daily) testing conditions.The testing was performed using two operators in eachlaboratory performing the test once on each of two days (totalof four tests). The pellet hardness average test result is theaverage of all the individual pellet har
29、dness values obtained ina single determination. The pellet hardness maximum testresult is the highest individual value of all the individual pellethardness values obtained in a single determination. Othertechniques for obtaining a maximum value, such as the averageof x number of the highest individu
30、al values or the average ofthe highest individual values that represent y percent of thetotal number of pellets tested are not included in theseprecision calculations. Acceptable difference values were notmeasured. The between operator component of variation isincluded in the calculated values for r
31、, (r), R, and (R).10.4 The results of the precision calculations for this testmethod are given in Tables 1-4. The materials are arranged inascending “mean level” order.10.5 RepeatabilityThe pooled relative repeatability, (r),for the pellet hardness average result of this test when testing20 pellets
32、has been established as 18.7 % (see Table 1). Thepooled relative repeatability, (r), for the pellet hardness aver-age result of this test when testing 50 pellets has beenestablished as 16.4 % (see Table 2). The pooled relativerepeatability, (r), for the pellet hardness maximum result of thistest whe
33、n testing 20 pellets has been established as 27.1 % (seeTable 3). The pooled relative repeatability, (r), for the pellethardness maximum result of this test when testing 50 pelletshas been established as 26.1 % (see Table 4). The best estimateof the test precision is given by the pooled values and t
34、heseD5230 1412should be used unless there is a good reason to use a differentvalue. Any other value in Tables 1-4 may be used as anestimate of repeatability, if justified, such as when testing thesame material as, or a material similar to, those in the tables.The difference between two single test r
35、esults (or determina-tions) found on identical test material under the repeatabilityconditions prescribed for this test will exceed the repeatabilityvalue on an average of not more than once in 20 cases in thenormal and correct operation of the method. Two single testresults that differ by more than
36、 the appropriate value fromTables 1-4 must be suspected of being from different popula-tions and some appropriate action taken.NOTE 2See footnote A in Table 3 and Table 4 concerning the validityof drawing any conclusions regarding the precision of the pellet hardnessmaximum test result.NOTE 3Appropr
37、iate 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 ReproducibilityThe pooled relative reproducibility,(R), for the pellet hardnes
38、s average result of this test whentesting 20 pellets has been established as 38.1 % (see Table 1).The pooled relative reproducibility, (R), for the pellet hardnessaverage result of this test when testing 50 pellets has beenestablished as 36.5 % (see Table 2). The pooled relativereproducibility, (R),
39、 for the pellet hardness maximum result ofthis test when testing 20 pellets has been established as 42.2 %(see Table 3). The pooled relative reproducibility, (R), for thepellet hardness maximum result of this test when testing 50pellets has been established as 46.0 % (see Table 4). The bestestimate
40、of the test precision is given by the pooled values andthese should be used unless there is a good reason to use adifferent value. Any other value in Tables 1-4 may be used asan estimate of reproducibility, if justified, such as when testingthe same material as, or a material similar to, those in th
41、etables. The difference between two single and independent testresults found by two operators working under the prescribedreproducibility conditions in different laboratories on identicaltest material will exceed the reproducibility value on anaverage of not more than once in 20 cases in the normal
42、andcorrect operation of the method. Two single test resultsTABLE 1 Precision Parameters for Test Method D5230, Pellet Hardness Average for 20 Pellets, (Type 1 Precision)Units cN (gf)MaterialNominalTestingPeriodNumber ofLaboratories(M/H/L)AMean Level Sr r (r) SR R (R)BSRB-8F Mar 2010 30(1/2/0) 19.3 1
43、.67 4.73 24.5 3.98 11.25 58.2SRB-8C Sep 2010 30(3/2/0) 23.9 1.55 4.38 18.4 2.10 5.95 24.9ITRB2 Mar 2011 22(2/2/0) 24.5 2.06 5.83 23.8 2.90 8.22 33.6N234 (Birla) Mar 2012 29(3/1/0) 25.4 2.09 5.92 23.3 2.54 7.17 28.2SRB-8E Sep 2008 16(1/0/0) 26.4 1.80 5.11 19.3 2.81 7.96 30.1N650 (Orion) Sep 2012 21(1
44、/1/0) 30.1 2.08 5.88 19.5 3.13 8.87 29.5SRB-8D Mar 2009 23(1/3/0) 35.3 2.39 6.77 19.2 7.02 19.88 56.4SRB-8B Jun 2009 28(1/2/0) 36.2 2.35 6.66 18.4 3.98 11.27 31.2SRB-8A Sep 2011 27(2/2/0) 36.9 1.97 5.57 15.1 4.19 11.86 32.2SRB-8A Mar 2008 19(1/1/0) 38.4 2.35 6.65 17.3 5.21 14.75 38.4N550 (Cabot) Sep
45、 2013 34(2/3/0) 41.1 2.18 6.16 15.0 5.69 16.10 39.1SRB-8A2 Mar 2013 36(3/3/0) 42.6 2.38 6.73 15.8 4.77 13.51 31.7Average 31.7Pooled Values 2.09 5.92 18.7 4.26 12.06 38.1AM=Mean outliers; H=High variability outliers; L=Low variability outliers. For a 1-sided k test there are no low outliers.BPreferre
46、d parameter shown in bold.TABLE 2 Precision Parameters for Test Method D5230, Pellet Hardness Average for 50 Pellets, (Type 1 Precision)Units cN (gf)MaterialNominalTestingPeriodNumber ofLaboratories(M/H/L)AMean Level Sr r (r)BSR R (R)BSRB-8F Mar 2010 22(1/2/0) 19.7 1.13 3.19 16.2 2.37 6.71 34.1SRB-8
47、C Sep 2010 24(1/3/0) 23.6 1.20 3.40 14.4 3.64 10.31 43.6ITRB2 Mar 2011 21(1/1/0) 24.2 1.67 4.73 19.5 3.55 10.04 41.4N234 (Birla) Mar 2012 21(1/1/0) 25.9 1.79 5.06 19.5 2.86 8.08 31.2SRB-8E Sep 2008 23(3/3/0) 26.9 1.64 4.64 17.3 2.84 8.04 29.9N650 (Orion) Sep 2012 23(1/2/0) 31.8 1.65 4.67 14.7 3.10 8
48、.77 27.6SRB-8D Mar 2009 16(1/1/0) 32.9 2.65 7.49 22.8 6.45 18.26 55.5SRB-8B Jun 2009 22(2/2/0) 37.1 1.83 5.17 13.9 2.99 8.47 22.8SRB-8A Sep 2011 24(1/1/0) 37.8 1.62 4.57 12.1 5.04 14.25 37.7SRB-8A Mar 2008 22(1/2/0) 40.1 2.04 5.78 14.4 4.33 12.26 30.6N550 (Cabot) Sep 2013 23(0/2/0) 42.1 2.04 5.78 13
49、.7 6.13 17.34 41.2SRB-8A2 Mar 2013 23(1/1/0) 45.6 2.52 7.14 15.7 4.38 12.40 27.2Average 32.3Pooled Values 1.87 5.28 16.4 4.17 11.80 36.5AM=Mean outliers; H=High variability outliers; L=Low variability outliers. For a 1-sided k test there are no low outliers.BPreferred parameter shown in bold.D5230 1413produced in different laboratories that differ by more than theappropriate value from Tables 1-4 must be suspected of beingfrom different populations and some appropriate investigativeor technical/commercial action taken.NOTE 4See footnote A in Table 3 and Ta
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