1、Designation: D5230 13D5230 14Standard 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 revis
2、ion. 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 tes
3、ter.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 a
4、ppropriate 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 BlackS
5、ampling 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 Asample of carbon black is passed through two sieves to isolate
6、 a fraction of uniform size.An appropriate amount of pelletsfrom this portion is selected and placed into the tester. The individual pellets are pressed against a platen with a load cell formeasuring force. As pressure is applied the pellet will either break with a rapid force reduction or the pelle
7、t will simply compress.The individual 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 character
8、istics.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 Jan. 1, 2013Sept. 1, 2014. Published February 2013October 2014. Originally approve
11、d in 1992. Last previous edition approved in 20122013 asD5230 12a.D5230 13. DOI: 10.1520/D5230-13.10.1520/D5230-14.2 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,TX 79065, E-mail: http
12、:/. 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 carefulconsideration at a
13、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 Summary page on the ASTM
14、 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 recommends that users consult
15、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 automatic loading of
16、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 at a constant rate,5.
17、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 instrument through the test
18、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 individual test end point (
19、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 Section 9, and5.1.8 A mea
20、ns 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 be segregated in a 12/
21、+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 samples in accordance with
22、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 criteria.7.2.2 Force dro
23、p. 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 aredetermined by agreement bet
24、ween 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, 0.801.44 mm.8. Procedure8.1
25、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 the No. 14 sieve, or to
26、 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 hammer operating.8.2
27、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 manual.9. Report9.1 Repo
28、rt 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 tested, and9.1.5 Size of
29、sieves used to prepare the sample.D5230 14210. 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 section give an estimate of
30、 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 particularmaterials an
31、d 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 2Tables 1-4. Both repeatability andreproducibility represent short term (daily) testing conditions. The testing was
32、performed using two operators in each laboratoryperforming the test once on each of two days (total of four tests). A The pellet hardness average test result is the average of allthe individual pellet hardness values obtained in a single determination. The pellet hardness maximum test result is the
33、highestindividual value of all the individual pellet hardness values obtained in a single determination. Other techniques for obtaining amaximum value, such as the average of x number of the highest individual values or the average of the highest individual valuesthat represent y percent of the tota
34、l number of pellets tested are not included in these precision calculations. Acceptable differencevalues were not measured. The between operator component of variation is included in the calculated values for r and R.r, (r), R,and (R).10.4 The results of the precision calculations for this test meth
35、od are given in Table 1Tables 1-4. The materials are arrangedin ascending “mean level” order.10.5 RepeatabilityThe pooled relative repeatability, (r), for the pellet hardness average result of this test when testing 20pellets has been established as 5 %. 18.7 % (see Table 1). The pooled relative rep
36、eatability, (r), for the pellet hardness averageresult of this test when testing 50 pellets has been established as 16.4 % (see Table 2). The pooled relative repeatability, (r), forthe pellet hardness maximum result of this test when testing 20 pellets has been established as 27.1 % (see Table 3). T
37、he pooledrelative repeatability, (r), for the pellet hardness maximum result of this test when testing 50 pellets has been established as 26.1% (see Table 4). The best estimate of the test precision is given by the pooled values and these should be used unless there is agood reason to use a differen
38、t value. Any other value in Table 1Tables 1-4 may be used as an estimate of repeatability, asappropriate. if justified, such as when testing the same material as, or a material similar to, those in the tables. The differencebetween two single test results (or determinations) found on identical test
39、material under the repeatability conditions prescribedfor this test will exceed the repeatability value on an average of not more than once in 20 cases in the normal and correct operationof the method. Two single test results that differ by more than the appropriate value from Table 1Tables 1-4 must
40、 be suspected ofbeing from different populations and some appropriate action taken.NOTE 2See footnote A in Table 3 and Table 4 concerning the validity of drawing any conclusions regarding the precision of the pellet hardnessmaximum test result.NOTE 3Appropriate action may be an investigation of the
41、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), for the pellet hardness average result of this test when testi
42、ng20 pellets has been established as 14 %. 38.1 % (see Table 1). The pooled relative reproducibility, (R), for the pellet hardnessaverage result of this test when testing 50 pellets has been established as 36.5 % (see Table 2). The pooled relative reproducibility,(R), for the pellet hardness maximum
43、 result of this test when testing 20 pellets has been established as 42.2 % (see Table 3). TheTABLE 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)B SR R
44、(R)BSRB-8F Mar 2010 22(1/2/0) 19.7 1.13 3.19 16.2 2.37 6.71 34.1SRB-8C 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 2.8
45、4 8.04 29.9N650 (Orion) Sep 2012 23(1/2/0) 31.8 1.65 4.67 14.7 3.10 8.77 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
46、14.4 4.33 12.26 30.6N550 (Cabot) Sep 2013 23(0/2/0) 42.1 2.04 5.78 13.7 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
47、 there are no low outliers.BPreferred parameter shown in bold.D5230 143pooled relative reproducibility, (R), for the pellet hardness maximum result of this test when testing 50 pellets has been establishedas 46.0 % (see Table 4). The best estimate of the test precision is given by the pooled values
48、and these should be used unless thereis a good reason to use a different value. Any other value in Table 1Tables 1-4 may be used as an estimate of reproducibility, asappropriate. if justified, such as when testing the same material as, or a material similar to, those in the tables. The differencebet
49、ween two single and independent test results found by two operators working under the prescribed reproducibility conditionsin different laboratories on identical test material will exceed the reproducibility value on an average of not more than once in 20cases in the normal and correct operation of the method. Two single test results produced in different laboratories that differ byTABLE 3 Precision Parameters for Test Method D5230, Pellet Hardness MaximumA for 20 Pellets, (Type 1 Precision)Units cN (gf)MaterialNominalTestingPeriodNumber
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