1、Designation: D 1511 00 (Reapproved 2006)Standard Test Method forCarbon BlackPellet Size Distribution1This standard is issued under the fixed designation D 1511; 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 (e) 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
3、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 appro-priate safety and health practices
4、and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 1799 Practice for Carbon BlackSampling PackagedShipmentsD 1900 Practice for Carbon BlackSampling Bulk Ship-mentsD 4483 Practice for Evaluating Precision for Test MethodStandards in th
5、e Rubber and Carbon Black ManufacturingIndustriesD 5817 Practice for Carbon Black, PelletedReduction,Blending, and Drying of Gross Samples for TestingE11 Specification for Wire Cloth and Sieves for TestingPurposes3. Significance and Use3.1 The variation in the size of the pellets may relate to thele
6、vel 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.4. Apparatus4.1 Riffle Sample Splitter as specified in Practice D 5817.4.2 Balance with a sensitivity of 0.1 g.4.3 Sieve
7、sU.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.4.4 Bottom receiver pan and top sieve cover
8、.4.5 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 distribution of pelle
9、tedcarbon black.4.5.1 Mechanical Sieve Shaker3The Ro-Tap Siever im-parts a uniform rotary and tapping motion to a stack of sievesas described in 4.3. 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 raps/min and 2
10、80 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 1/16 in.).
11、4.5.2 Vibratory Siever4The Retsch Sieve Shaker AS200has variable timer and amplitude settings. When set at 3 minand 0.5 amplitude, the AS200 provides satisfactory results. Itaccommodates a stack of sieves as described in 4.3.4.5.3 Automatic Sieve Shaker5The Gradex 2000 auto-matically performs all of
12、 the required steps including the1This 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, 2006. Published July 2006. Originally approvedin 1957. Last prev
13、ious edition approved in 2000 as D 1511 00e2.2For 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 source
14、 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 meeting of t
15、he responsible technical committee,1whichyou may attend.4The sole source of supply of the Retsch Sieve Shaker AS200 known to thecommittee at this time is Retsch Inc., 74 Walker Lane, Newtown, PA18940, E-mail:. If you are aware of alternative suppliers, please provide thisinformation to ASTM Internat
16、ional Headquarters. Your comments will receivecareful consideration at a meeting of the responsible technical committee,1whichyou may attend.5The sole source of supply of the Gradex 2000 known to the committee at thistime is Rotex, Inc., 1230 Knowlton Street, Cincinnati, OH 45223, E-mail:. If you ar
17、e 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.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Consho
18、hocken, PA 19428-2959, United States.weighing of the sample and the individual fractions retained oneach sieve. The equipment consists of a balance, autofeedsystem, electric motor that imparts a uniform rotary motion,pneumatically operated rods to provide the tapping action, andcomputer and software
19、 to record and perform analyses. Shaketime of 1 min provides satisfactory test results. The test sievesare described in 4.3.NOTE 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 install
20、ed to provideadditional tapping action.5. Sampling5.1 Lot samples shall be taken in accordance with PracticesD 1799 or D 1900.5.2 Practice D 5817 shall be used for blending or reducingsamples.6. Procedure6.1 Prepare carbon black for testing as noted in Section 5.NOTE 3It is not good practice to weig
21、h out the test portion by pouringit directly from the sample container since the smaller pellets will tend toremain in the container while the larger pellets pour out first. Dipping theblack from the container is the preferred technique.6.2 Prepare the sieve assembly by stacking the sieves in thefol
22、lowing 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 cover is not needed for the Gradex 2000.6.3 Mechanical and Vibratory Sieve Shakers6.3.1 Weigh 100.0 g of carbon black.6.3.2 Transfer weighed carbon black to the top sieve
23、.6.3.3 Install the sieve cover and transfer the sieve assemblyto the shaker. The stack in the shaker should be adjusted toeliminate looseness.6.3.4 Start the shaker and allow it to shake as noted below:6.3.4.1 Mechanical Shaker1 min with hammer operating.6.3.4.2 Vibratory Shaker3 min and 0.5 mm ampl
24、itude.6.3.5 Remove the sieve assembly from the apparatus andweigh individually the carbon black retained on each sieve andbottom receiver pan to the nearest 0.1 g.6.3.6 Record the data and calculate as noted in Section 7.6.4 Automatic Sieve Shaker6.4.1 Follow the manufacturers instructions to load s
25、oft-ware and configure the shake time to 1 min.6.4.2 Transfer the sieve assembly to the automatic sieveshaker.6.4.3 Weigh or measure approximately 100 g of carbonblack.6.4.4 Transfer measured carbon black to the autofeed con-tainer.6.4.5 Enter the sample identification into the operatingprogram. Rep
26、eat steps 6.4.3-6.4.5 as required for consecutivesamples. Up to six samples may be identified at one time.6.4.6 Start the testing sequence according to the manufac-turers operating instructions.6.4.7 Retrieve report from the computer.7. Calculation7.1 Calculate the pellet size distribution of the sa
27、mple to thenearest 0.1 % as follows:Sieve No. Mass Retained, g Percent Retained10 _ _18 _ _35 _ _60 _ _120 _ _Pan _ _Total _ _8. Report8.1 Report the following information:8.1.1 Proper identification of the sample,8.1.2 Result obtained from a single determination, reportedto the nearest 0.1 %.8.1.3
28、Apparatus used to determine test values.9. Precision and Bias69.1 This precision and bias section has been prepared inaccordance with Practice D 4483. Refer to Practice D 4483 forterminology and other statistical details.9.2 The precision results in this precision and bias give anestimate of the pre
29、cision described as follows. The precisionparameters should not be used for acceptance/rejection testingof materials without documentation that they are applicable tothose particular materials and the specific testing protocols thatinclude this test method.9.3 A Type 1 inter-laboratory precision pro
30、gram was con-ducted in 1988 to determine the testing precision of threesamples (Sample 1, Sample 2, and Sample 3) according to thistest method. Both repeatability and reproducibility representshort term testing conditions. The program was conducted byseven laboratories testing three samples twice on
31、 each of twodifferent days. A test result is the value obtained from a singledetermination. Acceptable differences were not measured.9.4 RepeatabilityThe repeatability, r, of the specificscreen fraction has been established as the value tabulated inTables 1-6. Two single test results (or determinati
32、ons) thatdiffer by more than r must be considered suspect and dictatesthat some appropriate investigative action be taken.9.5 ReproducibilityThe reproducibility, R, of the specificscreen fraction has been established as the value tabulated inTables 1-6. Two single test results (or determinations) th
33、atdiffer by more than R must be considered suspect and dictatesthat some appropriate investigative action be taken.9.6 BiasBias 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 th
34、e test property is exclusively defined by the test method.Therefore, bias cannot be determined.10. Keywords10.1 carbon black; pellet size distribution6Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR: D24-1007.D 1511 00 (2006)2TAB
35、LE 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 3.75 106.64pooled oraveragevalues 1
36、.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 standard deviation,R = reproducib
37、ility (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 2.14 6.06 13.39 7.50 21.21 46.8
38、5Sample 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 measured units),(r) = repeatability
39、 (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) SR R (R)Sample 3 20.66 1.43 4.
40、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:Sr = Within laboratory standard
41、 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+60AMaterialMeanLevel,%Within Labo
42、ratories 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 precision (days) with:p =7,q = 3, an
43、d 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 percent).TABLE 5 Precision-Type 1 Ca
44、rbon Black-Pellet Size Distribution+120AMaterialMeanLevel,%Within Laboratories Between LaboratoriesSr r (r) SR R (R)Sample 3 1.21 0.32 0.90 74.25 0.41 1.15 94.53Sample 1 4.97 0.72 2.04 40.95 1.84 5.20 104.55Sample 2 6.25 0.70 1.97 31.59 1.87 5.30 84.80pooled oraveragevalues 4.14 0.61 1.72 41.45 1.53
45、 4.34 104.63AThis 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 standard deviation,R = reproducibility (in measured units
46、), and(R) = reproducibility (in percent).D 1511 00 (2006)3ASTM 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 pate
47、nt 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 not revised, either reapproved or withdrawn. Your comments are invited eith
48、er 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 committee, which you may attend. If you feel that your comments have not received a fair h
49、earing 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 o
