1、Designation: D 3313 05aStandard Test Method forCarbon BlackIndividual Pellet Hardness1This standard is issued under the fixed designation D 3313; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number i
2、n parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers a method for measuring thehardness of individual pellets of carbon black.1.2 The values stated in SI units are to be r
3、egarded 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 appro-priate safety and health practices and det
4、ermine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 1511 Test Method for Carbon BlackPellet Size Distri-butionD 1799 Practice for Carbon BlackSampling PackagedShipmentsD 1900 Practice for Carbon BlackSampling Bulk Ship-mentsD 4483 Practice fo
5、r Evaluating Precision for Test MethodStandards in the Rubber and Carbon Black ManufacturingIndustriesD 5230 Test Method for Carbon BlackAutomated Indi-vidual Pellet HardnessE11 Specification for Wire Cloth and Sieves for TestingPurposes3. Significance and Use3.1 Pellet hardness is related to severa
6、l 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 agreed to by theuser and the producer.NOTE 1Test Method
7、D 5230 is the preferred standard for testing ofindividual pellet hardness. It is recognized that Test Method D 3313 relieson operator judgement, thus adding an additional source of variation forthis test.4. Summary of Test Method4.1 A sample of carbon black is passed through two sievesto isolate a f
8、raction 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.5. Apparatus5.1 Pellet-Hardness Tester,3of a type capable of measuringthe pellet ha
9、rdness 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 applying force at a constant rate,5.1.
10、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 transparentfoot mounted so it can be move
11、d directly over the pellet will serve toconvert a balance to a pellet hardness tester, as needed.5.2 Mechanical Sieve Shaker,4(see Test Method D 1511).1This test method is under the jurisdiction of ASTM Committee D24 on CarbonBlack and is the direct responsibility of Subcommittee D24.51 on Carbon Bl
12、ackPellet Properties.Current edition approved Dec. 1, 2005. Published January 2006. Originallyapproved in 1974. Last previous edition approved in 2005 as D 3313 05.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Boo
13、k of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3The sole source of supply of the pellet-hardness tester (Model-S Pellet StrengthTester with lab jack) known to the committee at this time is A. L. Sweigart,Technical Service Shop, 1206 Hemlock St.
14、, Borger, TX 79007. If you are aware ofalternative suppliers, please provide this information to ASTM InternationalHeadquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee,1which you may attend.4The sole source of supply of the mechanical siev
15、e shaker (Ro-Tap) known tothe committee at this time is W. S. Tyler, 8570 Tyler Blvd., Mentor, OH 44060. Ifyou are aware of alternative suppliers, please provide this information to ASTMInternational Headquarters. Your comments will receive careful consideration at ameeting of the responsible techni
16、cal committee,1which you may attend.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5.3 SievesU.S. Standard sieves or equivalents, conform-ing to Specification E11. Sieve Nos. 12 (1700-m) and 14(1400-m) shall be used.5.4 Bottom-Recei
17、ver 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.6. Sampling6.1 Samples shall be taken in accordance with PracticesD 1799 or D 1900.7. Calibration7.1
18、 Equipment 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 th
19、e bottom.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 t
20、he assembly 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 spheric
21、al pellets 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 individ
22、ual pellets, 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. T
23、his step 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
24、 8.5-8.7 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 individua
25、l value 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 D 4483. Refer to this practi
26、ce for termi-nology 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 areapplica
27、ble to 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,
28、 E, and 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 t
29、he pooled 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 di
30、ctates that someappropriate investigative action be taken.TABLE 1 ASTM Test Method Precision: Type 1 Carbon BlackIndividual Pellet Hardness (D 3313)ASymbols are defined as follows:Sr = within laboratory standard deviation,(r) = repeatability (in percent),SR = between laboratory standard deviation, a
31、nd(R) = reproducibility (in percent).Material Mean Level, cNWithin Laboratories Between Laboratoriessr (r) SR (R)D 21.4 2.64 34.8 6.20 81.8E 39.0 3.41 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 74.0AThis is short-term precision (days).D 3313 05a210.5.2 Repro
32、ducibilityThe 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 consideredsuspect and dictates that some appropriate investigative ortechn
33、ical/commercial action be taken.10.6 BiasIn test method terminology, bias is the differ-ence between 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 me
34、thod. Bias, 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 th
35、is 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 reviewed every five ye
36、ars 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 technical commi
37、ttee, 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 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 (e-mail); or through the ASTM website(www.astm.org).D 3313 05a3
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