1、Designation: D3313 121Standard Test Method forCarbon BlackIndividual Pellet Hardness1This standard is issued under the fixed designation D3313; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number in
2、parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1NOTECorrected 5.1 editorially in October 2016.1. Scope1.1 This test method covers a method for measuring thehardness of individual pellets of carbon black.1
3、.2 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for informationonly.1.3 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appr
4、o-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 PackagedShipmentsD1900 Practice for Carbon BlackS
5、ampling Bulk Ship-mentsD4483 Practice for Evaluating Precision for Test MethodStandards in the Rubber and Carbon Black ManufacturingIndustriesD5230 Test Method for Carbon BlackAutomated Indi-vidual Pellet HardnessE11 Specification for Woven Wire Test Sieve Cloth and TestSieves3. Summary of Test Meth
6、od3.1 A sample of carbon black is passed through two sievesto isolate a fraction of uniform size. The most spherical pelletsfrom this portion are selected and brought into contact with ameasuring device as force is applied. Pellet hardness is themaximum force required to crush the pellets.4. Signifi
7、cance and Use4.1 Pellet hardness is related to several carbon black char-acteristics. Among these are mass strength and attrition. Thesubsequent level of dispersion obtained in some mixed com-pounds containing the carbon black may be affected by pellethardness. Acceptable pellet hardness must be agr
8、eed to by theuser and the producer.NOTE 1Test Method D5230 is the preferred standard for testing ofindividual pellet hardness. It is recognized that Test Method D3313 relieson operator judgement, thus adding an additional source of variation forthis test.5. Apparatus5.1 Pellet-Hardness Tester, of a
9、type capable of measuringthe pellet hardness of the individual pellet in grams-force(centinewtons). A suitable tester must exhibit the followingcharacteristics:5.1.1 Initial contact force must be applied so that the forcearea rests lightly on the pellet before proceeding,5.1.2 It must be capable of
10、applying force at a constant rate,5.1.3 It must possess an accurate means of measuring theapplied force, and5.1.4 During the test, the applied force and base plate mustbe controlled so as not to cause the pellet to move or roll priorto crushing.NOTE 2A two-pan torsion balance with 100-g dial and tra
11、nsparentfoot mounted so it can be moved directly over the pellet will serve toconvert a balance to a pellet hardness tester, as needed.5.2 Mechanical Sieve Shaker, conforming to Test MethodD1511.5.3 SievesU.S. Standard sieves or equivalents, conform-ing to Specification E11. Sieve Nos. 12 (1700-m) a
12、nd 14(1400-m) shall be used.5.4 Bottom-Receiver Pan and Top-Sieve Cover.5.5 Container, shallow, flat approximately 305 mm (12 in.)long.5.6 Forceps, fitted with sponge tips. A very low-densityurethane foam sponge has been found to be acceptable.1This test method is under the jurisdiction of ASTM Comm
13、ittee D24 on CarbonBlack and is the direct responsibility of Subcommittee D24.51 on Carbon BlackPellet Properties.Current edition approved June 1, 2012. Published September 2012. Originallyapproved in 1974. Last previous edition approved in 2005 as D3313 05a. DOI:10.1520/D3313-12E01.2For referenced
14、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 Drive, PO Box C700, West Consho
15、hocken, PA 19428-2959. United StatesNOTICE: This standard has either been superseded and replaced by a new version or withdrawn.Contact ASTM International (www.astm.org) for the latest information16. Sampling6.1 Samples shall be taken in accordance with PracticesD1799 or D1900.7. Calibration7.1 Equi
16、pment used for this test shall be calibrated by deadweights or a force-measuring device that will verify theaccuracy of the equipment over the range to be tested.8. Procedure8.1 Prepare a sample of carbon black, as follows:8.1.1 Stack the No. 12 above the No. 14 sieve with thereceiver pan on the bot
17、tom.NOTE 3It is permissible to use multiples of sieves to screen severalsamples simultaneously.8.1.2 Place the sample in the top sieve and install the cover.Transfer the assembly to the shaking device.8.1.3 Allow the sieve assembly to shake for 60, 0 +10 s,with the hammer operating.8.2 Remove the as
18、sembly from the shaking device. Selectthe more spherical pellets retained on the No. 14 sieve.8.3 The more spherical pellets may be selected by pouringapproximately2gofpellets retained on the No. 14 sieve intoone end of the shallow container. Tilt the container slightly tocause the most spherical pe
19、llets to roll to the opposite end.8.4 Take 20 or 50 of the most spherical pellets for testing.Twenty pellets are tested in normal applications. Fifty pelletsmay be tested for critical applications. Critical applications aredetermined by agreement between the customer and supplier.Handle individual p
20、ellets, when transported or positioned fortest, or both, with the sponge-tipped forceps.8.5 Position pellet to be tested on a solid vibration-freesurface so as to be near the center area of the applied force.8.6 Bring the measuring device in contact with the pellet,but do not apply any force. This s
21、tep is most important whentesting soft pellets, which tend to fracture immediately orprematurely due to impact on initial contact.8.7 Apply force at a constant rate of approximately 5 cN/s(g force/s) until the pellet is fractured. Record the indicatedvalue to the nearest whole number.8.8 Repeat 8.5
22、8.7 until the appropriate number of pelletshave been tested.9. Report9.1 Report the following information:9.1.1 Proper identification of the sample,9.1.2 Average value in centinewtons (grams-force) roundedto the nearest millinewton (nearest 0.1 gram-force),9.1.3 Maximum as the highest individual val
23、ue in centin-ewtons (grams-force) rounded to a whole number,9.1.4 Number of pellets tested, and9.1.5 Any other results as determined between the purchaserand the seller.10. Precision and Bias10.1 This precision and bias has been prepared in accor-dance with Practice D4483. Refer to this practice for
24、 terminol-ogy and other statistical details.10.2 The precision results in this precision and bias give anestimate of the precision as described below. The precisionparameters should not be used for acceptance/rejection testingof any group of materials without documentation that they areapplicable to
25、 those particular materials and the specific testingprotocols that include this test method.10.3 A Type 1 inter-laboratory precision program was con-ducted in 1990. Both repeatability and reproducibility repre-sent short term testing conditions. Seven laboratories testedthree carbon blacks (D, E, an
26、d F) twice on two different days.Atest result is the value obtained from an average of 20 pellets.Acceptable difference values were not measured.10.4 The result of the precision calculations were given inTable 1 with the material arranged in ascending “mean level”order.10.5 The precision for the poo
27、led values for individualpellet hardness may be expressed as follows:10.5.1 RepeatabilityThe repeatability, (r), of the indi-vidual pellet hardness result has been established as 26.4 %.Two single test results (or determinations) that differ by morethan 26.4 % must be considered suspect and dictates
28、 that someappropriate investigative action be taken.10.5.2 ReproducibilityThe reproducibility, (R), of the in-dividual pellet hardness result has been established as 74.1 %.Two single test results (or determinations) produced in separatelaboratories that differ by more than 74.1 % must be considered
29、suspect and dictates that some appropriate investigative ortechnical/commercial action be taken.TABLE 1 ASTM Test Method Precision: Type 1 Carbon BlackIndividual Pellet Hardness (D3313)AMaterial Mean Level, cNWithin Laboratories Between Laboratoriessr (r) SR (R)D 21.4 2.64 34.8 6.20 81.8E 39.0 3.41
30、24.6 10.2 74.1F 39.6 3.25 23.2 9.26 66.1pooled or average values 33.4 3.12 26.4 8.73 74.0Symbols are defined as follows:Sr = within laboratory standard deviation,(r) = repeatability (in percent),SR = between laboratory standard deviation, and(R) = reproducibility (in percent).AThis is short-term pre
31、cision (days).D3313 121210.6 BiasIn test method terminology, bias is the differencebetween an average test 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
32、, therefore, cannotbe determined.11. Keywords11.1 carbon black; dispersion level; individual pellet hard-ness; pellet hardness testerASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standar
33、d 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 reviewed every five years andif
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36、ited 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 photocopy the standard may also be secured from the Copyright Clearance Center, 222Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http:/ 1213
