1、Designation: D3313 05a D3313 12Standard 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 n
2、umber 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 method for measuring the hardness of individual pellets of carbon black.1.2 The values stated in SI units are
3、to be regarded as the standard. The values given 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 appropriate safety and health practice
4、s and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D1511 Test Method for Carbon BlackPellet Size DistributionD1799 Practice for Carbon BlackSampling Packaged ShipmentsD1900 Practice for Carbon BlackSampling Bulk ShipmentsD4483 Practice
5、for Evaluating Precision for Test Method Standards in the Rubber and Carbon Black Manufacturing IndustriesD5230 Test Method for Carbon BlackAutomated Individual Pellet HardnessE11 Specification for Woven Wire Test Sieve Cloth and Test Sieves3. Summary of Test Method3.1 A sample of carbon black is pa
6、ssed through two sieves to isolate a fraction of uniform size. The most spherical pellets fromthis portion are selected and brought into contact with a measuring device as force is applied. Pellet hardness is the maximum forcerequired to crush the pellets.4. Significance and Use4.1 Pellet hardness i
7、s related to several carbon black characteristics. 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.
8、NOTE 1Test Method D5230 is the preferred standard for testing of individual pellet hardness. It is recognized that Test Method D3313 relies onoperator judgement, thus adding an additional source of variation for this test.5. Apparatus5.1 Pellet-Hardness Tester,3of a type capable of measuring the pel
9、let hardness of the individual pellet in grams-force(centinewtons). A suitable tester must exhibit the following characteristics:5.1 Initial contact force must be applied so that the force area rests lightly on the pellet before proceeding,5.1 It must be capable of applying force at a constant rate,
10、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 Dec. 1, 2005June 1, 2012. Published January 2006September 2012. Originally approved in 1974. Last previ
11、ous edition approved in 2005 asD3313 05.D3313 05a. DOI: 10.1520/D3313-05A.10.1520/D3313-12.2 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
12、Summary page on the ASTM website.3 The sole source of supply of the pellet-hardness tester (Model-S Pellet Strength Tester with lab jack) apparatus (the HITEC IPHT) known to the committee at this timeis HITEC Luxembourg, 5 rue de LEglise, L-1458, Luxembourg, E-mail: infohitec.lu, http:/www.hitec.lu/
13、. (Some Model-S Pellet Strength Testers with lab jack may stillbe in use and are suitable. This unit was in the past available from A. L. Sweigart, Technical Service Shop, 1206 Hemlock St., Borger, TX 79007.79007.) If you are awareof alternative suppliers, please provide this information to ASTM Int
14、ernational Headquarters. Your comments will receive careful consideration at a meeting of the responsibletechnical committee,1 which you may attend.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 p
15、revious version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult 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
16、 International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States15.1 It must possess an accurate means of measuring the applied force, and5.1 During the test, the applied force and base plate must be controlled so as not to cause the pellet to move or roll prior to
17、crushing.NOTE 2A two-pan torsion balance with 100-g dial and transparent foot mounted so it can be moved directly over the pellet will serve to convert abalance to a pellet hardness tester, as needed.5.2 Mechanical Sieve Shaker, (see conforming to Test Method D1511)5.3 SievesU.S. Standard sieves or
18、equivalents, conforming to Specification E11. Sieve Nos. 12 (1700-m) and 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-density urethane foam sponge has been found t
19、o be acceptable.6. Sampling6.1 Samples shall be taken in accordance with Practices D1799 or D1900.7. Calibration7.1 Equipment used for this test shall be calibrated by dead weights or a force-measuring device that will verify the accuracyof the equipment over the range to be tested.8. Procedure8.1 P
20、repare a sample of carbon black, as follows:8.1 Stack the No. 12 above the No. 14 sieve with the receiver pan on the bottom.NOTE 3It is permissible to use multiples of sieves to screen several samples simultaneously.8.1 Place the sample in the top sieve and install the cover. Transfer the assembly t
21、o the shaking device.8.1 Allow the sieve assembly to shake for 60, 0 +10 s, with the hammer operating.8.2 Remove the assembly from the shaking device. Select the more spherical pellets retained on the No. 14 sieve.8.3 The more spherical pellets may be selected by pouring approximately 2 g of pellets
22、 retained on the No. 14 sieve into oneend of the shallow container. Tilt the container slightly to cause the most spherical 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 pellets maybe tested fo
23、r critical applications. Critical applications are determined by agreement between the customer and supplier. Handleindividual pellets, when transported or positioned for test, or both, with the sponge-tipped forceps.8.5 Position pellet to be tested on a solid vibration-free surface so as to be near
24、 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 step is most important when testingsoft pellets, which tend to fracture immediately or prematurely due to impact on initial contact.8.7 Apply force at a constant rate of
25、approximately 5 cN/s (g force/s) until the pellet is fractured. Record the indicated valueto the nearest whole number.8.8 Repeat 8.5-8.7 until the appropriate number of pellets have been tested.9. Report9.1 Report the following information:9.1 Proper identification of the sample,9.1 Average value in
26、 centinewtons (grams-force) rounded to the nearest millinewton (nearest 0.1 gram-force),9.1 Maximum as the highest individual value in centinewtons (grams-force) rounded to a whole number,9.1 Number of pellets tested, and9.1 Any other results as determined between the purchaser and the seller.10. Pr
27、ecision and Bias10.1 This precision and bias has been prepared in accordance with Practice D4483. Refer to this practice for terminology andother statistical details.10.2 The precision results in this precision and bias give an estimate of the precision as described below. The precisionparameters sh
28、ould not be used for acceptance/rejection testing of any group of materials without documentation that they areapplicable to those particular materials and the specific testing protocols that include this test method.D3313 12210.3 A Type 1 inter-laboratory precision program was conducted in 1990. Bo
29、th repeatability and reproducibility represent shortterm testing conditions. Seven laboratories tested three carbon blacks (D, E, and F) twice on two different days. A test result is thevalue obtained from an average of 20 pellets. Acceptable difference values were not measured.10.4 The result of th
30、e precision calculations were given in Table 1 with the material arranged in ascending “mean level” order.10.5 The precision for the pooled values for individual pellet hardness may be expressed as follows:10.5 RepeatabilityThe repeatability, (r), of the individual pellet hardness result has been es
31、tablished as 26.4 %. Two singletest results (or determinations) that differ by more than 26.4 % must be considered suspect and dictates that some appropriateinvestigative action be taken.10.5 ReproducibilityThe reproducibility, (R), of the individual pellet hardness result has been established as 74
32、.1 %. Twosingle test results (or determinations) produced in separate laboratories that differ by more than 74.1 % must be considered suspectand dictates that some appropriate investigative or technical/commercial action be taken.10.6 BiasIn test method terminology, bias is the difference between an
33、 average test value and the reference (true) test propertyvalue. Reference values do not exist for this 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; dispersion level; individua
34、l pellet hardness; 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 standard are expressly advised that determination of the validity of any such patent rights, and th
35、e 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 not revised, either reapproved or withdrawn. Your comments are invited either for revision o
36、f 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 committee, which you may attend. If you feel that your comments have not received a fair hearing you should
37、make 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 obtaine
38、d 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 ASTM website (www.astm.org/COPYRIGHT/).4 The sole source of supply
39、 of the mechanical sieve shaker (Ro-Tap) known to the committee at this time is W. S. Tyler, 8570 Tyler Blvd., Mentor, OH 44060. If you areaware of alternative suppliers, please provide this information to ASTM International Headquarters. Your comments will receive careful consideration at a meeting
40、 of theresponsible technical committee,1 which you may attend.TABLE 1 ASTM Test Method Precision: Type 1 Carbon BlackIndividual Pellet Hardness (D3313)AMaterial Mean Level, cN Within 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 74.0Symbols are defined as follows:Sr = within laboratory standard deviation,(r) = repeatability (in percent),SR = between laboratory standard deviation, and(R) = reproducibility (in percent).A This is short-term precision (days).D3313 123
