1、Designation: D1511 10Standard Test Method forCarbon BlackPellet Size Distribution1This standard is issued under the fixed designation D1511; 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 par
2、entheses 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 the determination of the pelletsize distribution of carbon black.1.2 The values stated in SI units are to be regarded as the
3、standard. 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 determine the app
4、lica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D1799 Practice for Carbon BlackSampling PackagedShipmentsD1900 Practice for Carbon BlackSampling Bulk Ship-mentsD4483 Practice for Evaluating Precision for Test MethodStandards in the Rubber and Carbon Blac
5、k ManufacturingIndustriesD5817 Practice for Carbon Black, PelletedReduction,Blending, and Drying of Gross Samples for TestingE11 Specification for Woven Wire Test Sieve Cloth and TestSieves3. Summary of Test Method3.1 A 100 g sample of carbon black is shaken for 1 min ina sieve shaker to sort the pe
6、llets in a sieve assembly composedof the following sieve sizes: No. 10 (2000 m), No. 18 (1000m), No. 35 (500 m), No. 60 (250 m), No. 120 (125 m), andpan. The mass retained on each sieve determines the pellet sizedistribution.4. Significance and Use4.1 The variation in the size of the pellets may rel
7、ate to thelevel of dispersion and to the ease of handling. Due to the manyother variables that influence dispersion and handling, thesignificance of pellet size must be determined by the user.5. Apparatus5.1 Riffle Sample Splitter as specified in Practice D5817.5.2 Balance with a sensitivity of 0.1
8、g.5.3 SievesU.S. Standard Sieves or equivalent, conformingto Specification E11. Sieve Nos. 10, 18, 35, 60, and 120,having openings respectively of 2000, 1000, 500, 250, and 125m, shall be used. The sieves shall be 25 mm (1 in.) in heightand 200 mm (8 in.) in diameter.5.4 Bottom receiver pan and top
9、sieve cover.5.5 Sieve ShakerAny equipment that will vibrate or shakea stack of sieves in a manner that will allow the pellets toseparate into size fractions without excessive pellet breakage.The following three types of shakers have been found satis-factory for determining the pellet size distributi
10、on of pelletedcarbon black.5.5.1 Mechanical Sieve Shaker3The Ro-Tap Siever im-parts a uniform rotary and tapping motion to a stack of sievesas described in 5.3. The shaker machine shall be powered withan electric motor producing 181 to 183 rads/s (1725 to1750 r/min). This will produce 140 to 160 rap
11、s/min and 280 to320 rotary motions/min. The cover plate shall be fitted with acork stopper that shall extend 3 to 9 mm (18 to38 in.) above themetal recess. Materials other than cork, such as rubber orwood, are unacceptable. The height of the RoTap hammer shallbe set at 3.30 cm 6 0.15 cm (15/16 in. 6
12、 1/16 in.).1This test method is under the jurisdiction of ASTM Committee D24 on CarbonBlack and is the direct responsibility of Subcommittee D24.51 on Carbon BlackPellet Properties.Current edition approved July 1, 2010. Published August 2010. Originallyapproved in 1957. Last previous edition approve
13、d in 2006 as D1511 00 (2006).DOI: 10.1520/D1511-10.2For 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.3The sole
14、source of supply of the Ro-Tap Siever known to the committee at thistime is WS Tyler, 8570 Tyler Blvd., Mentor, OH 44060, E-mail:. If you are aware of alternative suppliers, please provide thisinformation to ASTM International Headquarters. Your comments will receivecareful consideration at a meetin
15、g of the responsible technical committee,1whichyou may attend.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5.5.2 Vibratory Siever4The Retsch Sieve Shaker AS200has variable timer and amplitude settings. When set at 3 minand 0.5 amp
16、litude, the AS200 provides satisfactory results. Itaccommodates a stack of sieves as described in 5.3.5.5.3 Automatic Sieve Shaker5The Gradex 2000 auto-matically performs all of the required steps including theweighing of the sample and the individual fractions retained oneach sieve. The equipment c
17、onsists of a balance, autofeedsystem, electric motor that imparts a uniform rotary motion,pneumatically operated rods to provide the tapping action, andcomputer and software to record and perform analyses. Shaketime of 1 min provides satisfactory test results. The test sievesare described in 5.3.NOT
18、E 1Top sieve cover is not needed for the Gradex 2000.NOTE 2The Gradex is supplied with one standard tapping rod. It isrecommended that two additional tapping rods be installed to provideadditional tapping action.6. Sampling6.1 Lot samples shall be taken in accordance with PracticesD1799 or D1900.6.2
19、 Practice D5817 shall be used for blending or reducingsamples.7. Procedure7.1 Prepare carbon black for testing as noted in Section 6.NOTE 3It is not good practice to weigh out the test portion by pouringit directly from the sample container since the smaller pellets will tend toremain in the contain
20、er while the larger pellets pour out first. Dipping theblack from the container is the preferred technique.7.2 Prepare the sieve assembly by stacking the sieves in thefollowing order from bottom to top: Bottom receiver pan, No.120, No. 60, No. 35, No. 18, No. 10, and top sieve cover.NOTE 4Top sieve
21、cover is not needed for the Gradex 2000.7.3 Mechanical and Vibratory Sieve Shakers7.3.1 Weigh 100.0 g of carbon black.7.3.2 Transfer weighed carbon black to the top sieve.7.3.3 Install the sieve cover and transfer the sieve assemblyto the shaker. The stack in the shaker should be adjusted toeliminat
22、e looseness.7.3.4 Start the shaker and allow it to shake as noted below:7.3.4.1 Mechanical Shaker1 min with hammer operating.7.3.4.2 Vibratory Shaker3 min and 0.5 mm amplitude.7.3.5 Remove the sieve assembly from the apparatus andweigh individually the carbon black retained on each sieve andbottom r
23、eceiver pan to the nearest 0.1 g.7.3.6 Record the data and calculate as noted in Section 8.7.4 Automatic Sieve Shaker7.4.1 Follow the manufacturers instructions to load soft-ware and configure the shake time to 1 min.7.4.2 Transfer the sieve assembly to the automatic sieveshaker.7.4.3 Weigh or measu
24、re approximately 100 g of carbonblack.7.4.4 Transfer measured carbon black to the autofeed con-tainer.7.4.5 Enter the sample identification into the operatingprogram. Repeat steps 7.4.3-7.4.5 as required for consecutivesamples. Up to six samples may be identified at one time.7.4.6 Start the testing
25、sequence according to the manufac-turers operating instructions.7.4.7 Retrieve report from the computer.8. Calculation8.1 Calculate the pellet size distribution of the sample to thenearest 0.1 % as follows:Sieve No. Mass Retained, g Percent Retained10 _ _18 _ _35 _ _60 _ _120 _ _Pan _ _Total _ _9. R
26、eport9.1 Report the following information:9.1.1 Proper identification of the sample,9.1.2 Result obtained from a single determination, reportedto the nearest 0.1 %.9.1.3 Apparatus used to determine test values.10. Precision and Bias610.1 This precision and bias section has been prepared inaccordance
27、 with Practice D4483. Refer to Practice D4483 forterminology and other statistical details.10.2 The precision results in this precision and bias give anestimate of the precision described as follows. The precisionparameters should not be used for acceptance/rejection testingof materials without docu
28、mentation that they are applicable tothose particular materials and the specific testing protocols thatinclude this test method.10.3 A Type 1 inter-laboratory precision program was con-ducted in 1988 to determine the testing precision of threesamples (Sample 1, Sample 2, and Sample 3) according to t
29、histest method. Both repeatability and reproducibility representshort term testing conditions. The program was conducted byseven laboratories testing three samples twice on each of twodifferent days. A test result is the value obtained from a singledetermination. Acceptable differences were not meas
30、ured.10.4 RepeatabilityThe repeatability, r, of the specificscreen fraction has been established as the value tabulated inTables 1-6. Two single test results (or determinations) that4The sole source of supply of the Retsch Sieve Shaker AS200 known to thecommittee at this time is Retsch Inc., 74 Walk
31、er Lane, Newtown, PA18940, E-mail:. If you are aware of alternative suppliers, please provide thisinformation to ASTM International Headquarters. Your comments will receivecareful consideration at a meeting of the responsible technical committee,1whichyou may attend.5The sole source of supply of the
32、 Gradex 2000 known to the committee at thistime is Rotex, Inc., 1230 Knowlton Street, Cincinnati, OH 45223, E-mail:. If you are aware of alternative suppliers, please provide thisinformation to ASTM International Headquarters. Your comments will receivecareful consideration at a meeting of the respo
33、nsible technical committee,1whichyou may attend.6Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D24-1007.D1511 102differ by more than r must be considered suspect and dictatesthat some appropriate investigative action be taken.1
34、0.5 ReproducibilityThe reproducibility, R, of the specificscreen fraction has been established as the value tabulated inTables 1-6. Two single test results (or determinations) thatdiffer by more than R must be considered suspect and dictatesthat some appropriate investigative action be taken.10.6 Bi
35、asBias is the difference between an average testvalue and the reference (true) test property value. Referencevalues do not exist for this test method since the value or levelof the test property is exclusively defined by the test method.Therefore, bias cannot be determined.11. Keywords11.1 carbon bl
36、ack; pellet size distributionTABLE 1 Precision-Type 1 Carbon Black-Pellet Size Distribution+10AMaterialMeanLevel,%Within Laboratories Between LaboratoriesSr r (r) SR R (R)Sample 2 0.62 0.08 0.21 34.36 0.27 0.76 121.45Sample 3 1.77 0.23 0.64 36.08 0.49 1.39 78.37Sample 1 3.52 0.32 0.90 25.58 1.33 3.7
37、5 106.64pooled oraveragevalues 1.97 0.23 0.65 32.94 0.83 2.35 119.29AThis is short term precision (days) with:p =7,q = 3, and n =4.Symbols are defined as follows:Sr = Within laboratory standard deviation,r = repeatability (in measured units),(r) = repeatability (in percent),SR = Between laboratory s
38、tandard deviation,R = reproducibility (in measured units), and(R) = reproducibility (in percent).TABLE 2 Precision-Type 1 Carbon Black-Pellet Size Distribution+18AMaterialMeanLevel,%Within Laboratories Between LaboratoriesSr r (r) SR R (R)Sample 2 24.89 1.36 3.84 15.42 6.27 17.75 71.31Sample 1 45.27
39、 2.14 6.06 13.39 7.50 21.21 46.85Sample 3 72.75 2.34 6.63 9.11 2.98 8.43 11.59pooled oraveragevalues 47.64 1.99 5.64 11.84 5.90 16.69 35.04AThis is short term precision (days) with:p =7,q = 3, and n =4.Symbols are defined as follows:Sr = Within laboratory standard deviation,r = repeatability (in mea
40、sured units),(r) = repeatability (in percent),SR = Between laboratory standard deviation,R = reproducibility (in measured units), and(R) = reproducibility (in percent).TABLE 3 Precision-Type 1 Carbon Black-Pellet Size Distribution+35AMaterialMeanLevel,%Within Laboratories Between LaboratoriesSr r (r
41、) SR R (R)Sample 3 20.66 1.43 4.05 19.61 2.03 5.76 27.88Sample 1 32.48 1.03 2.91 8.96 5.70 16.13 49.65Sample 2 43.02 0.88 2.48 5.76 1.33 3.77 8.76pooled oraveragevalues 32.05 1.14 3.21 10.03 3.58 10.12 31.59AThis is short term precision (days) with:p =7,q = 3, and n =4.Symbols are defined as follows
42、:Sr = Within laboratory standard deviation,r = repeatability (in measured units),(r) = repeatability (in percent),SR = Between laboratory standard deviation,R = reproducibility (in measured units), and(R) = reproducibility (in percent).TABLE 4 Precision-Type 1 Carbon Black-Pellet Size Distribution+6
43、0AMaterialMeanLevel,%Within Laboratories Between LaboratoriesSr r (r) SR R (R)Sample 3 2.97 0.65 1.84 61.94 1.07 3.03 101.92Sample 1 11.90 1.22 3.45 28.97 3.28 9.29 78.04Sample 2 21.36 1.12 3.18 14.86 2.21 6.25 29.25pooled oraveragevalues 12.08 1.03 2.91 24.07 2.37 6.70 55.44AThis is short term prec
44、ision (days) with:p =7,q = 3, and n =4.Symbols are defined as follows:Sr = Within laboratory standard deviation,r = repeatability (in measured units),(r) = repeatability (in percent),SR = Between laboratory standard deviation,R = reproducibility (in measured units), and(R) = reproducibility (in perc
45、ent).D1511 103ASTM 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 the riskof infringement of su
46、ch 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 of this standard or for addi
47、tional 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 shouldmake your views known to th
48、e 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
49、 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/).TABLE 5 Precision-Type 1 Carbon Black-Pellet Size Distribution+120AMaterialMeanLevel,%Within Laboratories
